Supra-Clean® and Supra-Poly® Solid Phase Extraction (SPE) Application Notebook

FAST, EASY
EFFICIENT
SAMPLE PREPARATION

Supra-Clean® and Supra-Poly®
Solid Phase Extraction (SPE)
A Reference Notebook of SPE Applications

INTRODUCTION
AND OVERVIEW At PerkinElmer, we
understand that sample
preparation is one of the
most critical steps in the analytical process. Often accounting
for 60% of your timetable, it has a fundamental impact on a
wide range of operational parameters. Any errors within this
process undermine the quality of your data at all subsequent
stages of your analysis. Solid Phase Extraction (SPE) helps
avoid potential errors in sample preparation, reducing re-runs
and dramatically increasing productivity. As one of the most cost-effective and
flexible tools within the laboratory environment, SPE also provides efficient sample
concentration and purification prior to many of today’s most popular analytical
techniques, including HPLC, LC/MS, GC and GC/MS. This document is intended to
provide you with the tools you need to quickly and efficiently develop extraction
methods for your sampling analysis.
PerkinElmer SPE Solutions are ideal for a broad array of analytes and matrices.
We offer a variety of formats including Large Reservoir Capacity (LRC) columns,
Polypropylene (PP) columns, cartridges 96 well plate format, and glass columns. Each
technology is offered with a wide selection of polymer and silica sorbents. Varied
column capacities and bed weights allow you to perform scalable analyses depending
upon your sample size and required detection limits.
PerkinElmer® Supra-Clean® silica-based and Supra-Poly® polymer-based SPE cartridges
and columns.
Answering your needs. Empowering Your Lab.

www.perkinelmer.com/spe 3

TABLE OF CONTENTS

ENVIRONMENTAL
............................................................................................................................................... 12
............................................................................................................................ 13
........................................................................................................................................ 14
.............................................................................................................................................................. 15
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............................................................................................................................................................ 18
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............................................................................................................................ 21
..........................................................................................................................................22
.....................................................................................................................................................23
.................................................................................................................................................24 - 25

FORENSIC
..................................................................................................................................................26
............................................................27
...................................................................................................................................................28
....................................................................................................................29
....................................................................................................................................................30
......................................................................... 31
........................................................................32
................................................................................................33
...............................................34
..................................................................................................................................................................35
......................................................................................................................................36

PHARMACEUTICAL
...................................................................................................................................................37
.................................................................................................................................................38
...........................................................................................39
..........................................................................................................................40

4

TABLE OF CONTENTS

PHARMACEUTICAL
........................................................................................................................................................ 41
........................................................................................................................................42
.....................................................................43
.......................................................................................................................................................44
...................................................................................................................45
..............................................................................................................46
.........................................................................................................................................................47
........................................................................................................................... 48 - 50
............................................................................................................................................ 51
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.............................................................................................................................53
.................................................................................................................................................54
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...........................................................................................................................58


Supra-Clean and Supra-Poly Solid Phase Extraction (SPE)
Columns with Precise Bed Technology™

Supra-Clean and Supra-Poly SPE products are designed to offer you a sample
preparation solution that decreases your sample preparation time all while maintaining a
high level of reproducibility. Supra-Clean uses a silica based media and Supra-Poly uses

spherical particles, which allow columns to be evenly and consistently filled resulting in
optimum bed density.
Optimum bed density delivers a level of performance unattainable with the irregularly
shaped silica used in competitive solutions. The homogeneous filling and mono-
dispersed spherical media not only provide unparalleled reproducibility, it also delivers
superior performance.
Homogeneous filling and spherical media yield a +/- 1% variation in bed volume
precision, a significant improvement from the industry average. This level of quality
control allows customers to experience consistent sample preparation performance
column to column, batch to batch, and lot to lot.
Sample diffusion through Supra-Clean/Supra-Poly spherical media is also better than in
other systems, improving flow efficiency and avoiding channeling and clogging due to
fines. This enables smaller sample sizes to be used without compromising recovery levels,
dramatically reducing solvent volumes, analytical costs and processing times. This allows
you to work faster and more cost effectively, all while experiencing complete recovery,
reproducibility and reliability.

Precise Bed Technology

Weighing technology with +/- 1% accuracy
Guarantee of reproducibility from batch to batch & column to column

Bottom Polyethylene frit
Zero extractable

Polypropylene HMW tube
Zero extractable

Top Polyethylene frit
a special cut-off ensure a
perfect sample diffusion
without clogging
Optimum bed density Zero extractable

All columns are thoroughly quality control tested in-house to guarantee tracability. Products are supplied with an
individual certificate detailing the specific production number and sorbent batch.

6

Choose the Best SPE Solution For Your Method
To find the ideal SPE column for your particular application, simply follow the flow diagram below, selecting
your path based on the options at each junction.

Your Sample

Type of Matrix Aqueous Organic

Analyte Follow same path
Water Water Organic Solvents
Solubility as Organic

Ionic
Analyte Neutral (Follow same Ionic Neutral Neutral
path as Ionic
analyte)

Analyte Moderately Cationic Anionic
Non-Polar Polar Non-Polar Non-Polar Polar
Polarity Polar Bases Acids

Recommended Reversed Phase Ion Exchange Reversed Phase Normal Phase
Chromatography Chromatography Chromatography Chromatography Chromatography
Supra-Poly Extreme Capacity 1500 m2/g (XC)*
Supra-Clean Strong Anion Exchange (SAX)
Supra-Clean Mixed-Mode (MM3)

SPE Weak Cation Exchange (WCX)
SPE Strong Cation Exchange (SCX)

Supra-Poly 1200 m2/g (XWP)*
Supra-Poly (ATH, ATL, AEV)*

Supra-Clean Polyamine (P6)
Supra-Clean Amino (NH2-S)


Supra-Clean Phenyl (PH-S)

Supra-Clean Phenyl (PH-S)
Supra-Clean Cyano (CN-S)

Supra-Clean Florisil (FL-S)
Supra-Clean Silica (SI-S)
Supra-Clean 300Å C4

Supra-Clean 300Å C4
Supra-Clean REC18

Supra-Clean REC18
Supra-Clean C18

Supra-Clean C18
Supra-Clean LCC

Supra-Poly HLB

Supra-Poly HLB

Recommended
SPE Products

*AEV = Advanced Environmental HLB = Hydrophilic Lipophylic Balanced
ATH = Hydrophobic/Hydrophilic XC = Extreme Capacity
ATL = Lipophilic XWP = Extra Wide Particle


A Wide Array of Columns for a Broad Range of Applications
SUPRA-CLEAN SPHERICAL SILICA

Phase Mechanism Interaction mode Compounds Matrix
C18-S Hydrophobic Reversed Phase Polar to Non-Polar compounds Biological fluids, aqueous samples

High Recovery REC18 Hydrophobic Reversed Phase Non-polar and mid-polar compounds Biological fluids, aqueous samples
including 100% water solvents

Phenyl (PH-S) Hydrophobic Reversed Phase Non-polar to mid-polar Biological fluids
aromatic compounds
Silica (SI-S) Hydrophilic Normal Phase Polar compounds Non-polar organics,
oils, lipids

Amino (NH2-S) Hydrophilic Normal Phase Polar to Mid-Polar Biological fluids, aqueous samples,
aromatic compounds buffered organics
Strong Cation Ion Exchange Ion Exchange Basic compounds Biological fluids, aqueous samples,
Exchange (SCX) buffered organics

Weak cation Ion Exchange Ion Exchange Strong basic compounds Biological fluids, aqueous samples
Exchange (WCX)

Strong Anion Ion Exchange Ion Exchange Acidic compounds Biological fluids, aqueous samples
Exchange (SAX)
Cyano (CN-S) Hydrophilic Normal Phase Polar to Mid-Polar compounds Non-polar organics, oils, lipids
Florisil (FL-S) Hydrophilic Normal Phase Polar compounds Ideal for polar compounds in non-polar matrix

Florisil Pesticide (FL-S) Hydrophilic Normal Phase Polar compounds Ideal for polar compounds in non-polar matrix

Polyamine (P6) Hydrophilic Reversed Phase Carboxylic acids, phenolics Aqueous and mid-polar matrices
and nitroaromatics
300 A (C4) Hydrophobic Reversed Phase Non-polar to mid-polar compounds Biological Samples
LCC Hydrophobic Reversed Phase Non-polar to mid-polar compounds Biological fluids, aqueous samples
Mixed mode (MM1) Ion Exchange/ Hydrophobic Reversed Phase / SCX Basic compounds Biological samples
Mixed mode (MM2) Ion Exchange/ Hydrophobic Reversed Phase / WCX Very basic compounds Biological samples
Mixed mode (MM3) Ion Exchange/ Hydrophobic Reversed Phase / SAX Acidic compounds Biological samples

SUPRA-POLY SPHERICAL POLYMER
Extreme Capacity (XC) Hydrophobic Reversed Phase Polar and non-polar Aqueous or organic
Extreme Capacity Hydrophobic Reversed Phase Polar and non-polar Biological and viscous samples
Wide Pore (XWP)
Hydrophilic (ATH) Hydrophilic Reversed Phase Mid to non-polar compounds Aqueous or organic

Lipophilic (ATL) Lipophilic Reversed Phase Mid to non-polar compounds Crude samples

Environmental (AEV) Hydrophilic/ Hydrophobic Reversed Phase Mid to non-polar compounds Aqueous or Organic

HLB Hydrophilic/lipophilic balanced Reversed Phase Mid to non-polar compounds Aqueous or organic

8

pH End- Pore Surface Particle
Typical Applications Range capping Size (A) Area (m2/g) Size (um) Comments
Drugs and drug metabolites in 2-8 Yes 60 500 50 18% Carbon Load (CL)
biological matrices, trace organic material
in water, toxins in food
Drugs and drug metabolites in biological 2-8 Yes NA NA 50 High capacity and better recovery especially
matrices, trace organic material in water, for high acqueous conditions. 15% CL
toxins in food
Benzodiazepines in biological matrices, 2-8 No 60 500 50 9% CL
extraction of aromatic compounds
Aldehydes, amines, pesticides, herbicides, 2-8 No 60 500 50 Bare Silica
carotenoids, fat soluable vitamins, baflatoxins,
fatty acids, and phospholipids
Basic compounds, polar amine 2-8 No 60 500 50 5% CL
compounds, carbohydrates
Cations, antibiotics, drugs, amino acids, 2-8 No 60 450 60 Strong Acid - Sulfonic acid;;
catecholamines, herbicides, nucleic acid bases, Exchange capacity 0.70 meq/g
nucleosides, and surfactants
Cations, amines, antibiotics, drugs, amino acids, 2-8 No 60 450 60 Weak Acid - Carboxylic acid;; Exchange
catecholamines, nucleic acid bases, nucleosides, capacity 0.22 meq/g
and surfactants
Acidic food pigments, organic acids, phenol 2-8 No 60 450 60 Strong Base - quaternary amine;;
compounds, nucleic acids, nucleotides, surfactants Exchange capacity 0.30 meq/g
Polar compounds in hexane and oil 2-8 Yes 60 500 50 8% CL;; Mid-range polarity between silica and C18
Pesticides, Polychlorinated Biphenyls (PCB) 2-8 No NA NA 200 Standard grade. Alternative to silica for viscous
matrices due to large particle size. Granular shape
Pesticides 2-8 No NA NA 200 High purity pesticide grade. Alternative to silica
for viscous matrices. Granular shape
Aromatic and naturalproducts;; Flavones, 2-8 No NA NA 100 Nylon 6
Chalkones, Anthraquinones
Hydrophobic peptides and polypeptides 2-8 No 300 - - Large pore size for isolation of large biomolecules
Non-polar compounds in aqueous solution 2-8 Yes 60 500 50 10% CL;; Lower carbon load than C18-S and REC18
Drugs and drug metabolites 2-8 No 60 450 60 Exchange capacity 0.09 meq/g

Drugs and drug metabolites biological fluids 0-14 No NA 1500 70 High capacity polystyrene-divinylbenzene (PSDVB)
Drugs and drug metabolites biological fluids 0-14 No Wide Pore 1200 90 High capacity PSDVB for large biomolecules
and viscous matrices
Mid-polar and non-polar compounds in aqueous 1-13 No 70 800 75 Mixed hydrophilic/hydrophobic interactions
and organic solvents
Lipids 0-14 No 70 800 100 PSDVB;; Alternative to high flow silica for mid-polar
to non-polar compounds (<3000D) in crude samples
Aqueous environmental compounds that are 1-12 No 70 800 75 Advanced environmental;; Polystyrene-co-2-
not retained on C18 hydroxyethyl methacrylate (PSHEMA)
Mid-polar and non-polar compounds in 0-14 No 80 850 30 & 60 Hydrophilic-lipophilic-balanced reversed-
aqueous and organic solvents phase sorbent for acids, bases and neutrals


Six Steps for Clean Extract
1. Pretreat Sample
Some samples require initial pretreatment to obtain the optimal extraction. This pretreatment can include homoginization of solid samples, adjustment of the
matrix to the proper ionic strength and pH, and removal of particulates via filtration or centrifugation. This step may also include addition of an internal standard.

2. Condition Column
Sorbent activation and functional group activation are achieved by passing a volume of an appropriate solvent or a mixture of
solvent, through the column. Column frits are simultaneously conditioned as well.
Methanol or acetonitrile are commonly used for activating hydrophobic sorbents, while hexane or dichloromethane activate
hydrophilic sorbents. 2 to 4 bed volumes are typically recommended. See SPE Solvent Selection Guide (below).
Note: Once the conditioning is done never let the column dry unless it is specified in the method.
Load Sample
3. Load Sample
Apply your sample onto the upper part of the sorbent bed. Matrix contaminants may pass through the column unretained while
other matrix components may be more or less strongly retained on the sorbent surface.
To get a maximum purification efficiency, the sample flow needs to be controlled via vacuum or pressure. To achieve faster flow
of viscous sample through a column, 90 µμm sorbents or larger particle size can be used. The exchange capacity and selectivity
are unaffected.
Note: It is necessary to analyze the unretained fraction to check if all compounds of interest have been retained.

4. Wash Column
Passing solvents through columns washes away interfering compounds while leaving the analyte of interest undisturbed
on the sorbent bed.
Different solvents or solvent mixtures may be used to improve the rinsing efficiency. See SPE Solvent Selection Guide (below).

5. Dry Column (optional)
A drying step may be required. Solvent traces are evaporated by circulating air through the column over a 2 to 10 minute
time period. This improves the extraction yield for certain methods and compounds.

6. Elute Compounds of Interest
An appropriate solvent is passed through the column to disrupt the analyte-sorbent interaction and to elute 100% of
compounds of interest.
The appropriate solvent must have maximum interaction with the compound of interest and a minimal interaction
with the remaining impurities, leaving them undisturbed on the sorbent bed. See SPE Solvent Selection Guide (below).
In addition, the volume of the elution solvent needs to be as small as possible to maximize the concentration factor.
Note: Sorbent with low particle size (e.g 30, 50 µμm) gives a lower elution volume than larger sorbent particle size (e.g 90, 140 µμm).

SPE Solvent Selection Guide
The choice of solvent is dependent upon the
Carbon tetrachloride

sample matrix and the retention mechanism used.
Methylene Chloride

This table shows the differing polarities of
Petroleum Ether

Tetrahydrofuran

Ethyl Acetate

solvents commonly used in SPE.
Diethyl Ether
Cyclohexane

Isopropanol
Acetonitrile
Chloroform

Acetic Acid
Methanol
Isooctane

Acetone
Toluene

Pyridine

Ethanol
Hexane

Water

Solvent

NONPOLAR POLAR

Water Miscible No No No No No No No No Yes No Poor Yes Yes Yes Yes Yes Yes Yes Yes

10

Method Development for SPE
Imagine how much faster, easier and more efficient your method development would be if your Solid Phase Extraction (SPE) column
selection kits were designed to streamline your process. PerkinElmer has created column specific kits for some of the more common
analyses performed in today’s laboratories. These kits dramatically reduce set-up time for these methods and make it easy to select the
appropriate solution based on your specific matrices.

PerkinElmer SPE Column Selection Kits Media Weight Volume Qty. Part No.
Pre-Concentration of Hydrophobic Compounds from Aqueous Matrix 200 mg 6 mL 50 N9306594
200 mg 3 mL 50 N9306595
Type of matrix: aqueous
Principle: concentration of non-polar, mid-polar compounds
Includes 10 each: Supra-Clean C18 with cartridge, REC18;; Supra-Poly Lipophilic (ATL), extreme capacity (XC), hydrophobic/hydrophilic (ATH)

Extraction of Hydrophobic Compounds from Aqueous Matrix 500 mg 6 mL 50 N9306596
500 mg 3 mL 50 N9306597
Type of matrix: aqueous or (organics and aqueous) mixtures
Principle: extraction of non-polar and mid-polar compounds
Includes 10 each: Supra-Clean C18 (un-end-capped), C18 with cartridge, REC18, LCC, Phenyl

Pre-Concentration of Hydrophilic Compounds 500 mg 6 mL 30 N9306598
500 mg 3 mL 30 N9306599
Type of matrix: aqueous or (organics and aqueous) mixtures
Principle: extraction of non-polar and mid-polar compounds
Includes 10 each: Supra-Clean Amino, Cyano, Silica with cartridge

Removal of Polar Compounds from Aqueous and Organic Matrix 500 mg 6 mL 30 N9306600
500 mg 3 mL 30 N9306601
Type of matrix: aqueous or organics
Principle: Extraction and concentration of acidic, basic and neutral compounds

Extraction of Acidic Basic and Neutral Compounds from Aqueous or
Organic Matrix 100 mg 3 mL 50 N9306602
Type of matrix: aqueous or organics
Principle: Extraction and concentration of acidic, basic and neutral compounds
Includes 10 each: Supra-Poly Lipophilic (ATL), extra wide particle (XWP), extreme capacity (XC), advanced environmental (AEV),
hydrophobic/hydrophilic (ATH)

Extraction of Carboxylic Acids and Strong Bases from Aqueous Matrix 500 mg 6 mL 40 N9306603
Principle: selective extraction of weak acids and strong bases with the same protocol
Includes 10 each: Supra-Clean Strong Anion Exchange, Weak Cation Exchange, Mixed-Mode 2, 3

Extraction of Weak Bases from Aqueous Matrix 500 mg 6 mL 30 N9306604
Principle: extraction of weak bases
Includes 15 each: Supra-Clean Strong Cation Exchange, Mixed-Mode 1


ENVIRONMENTAL
2,4-Dichlorophenol in Water
PerkinElmer SPE Supra-Poly XC 500 mg/6 mL, Plastic Tube (Straight) Part No. N9306405

SAMPLE PRETREATMENT ELUTION
Adjust pH to 2 with H2SO4 3 mL tetrahydrofuran

COLUMN CONDITIONING CONCENTRATION
5 mL methanol Concentrate sample to 3 mL under nitrogen
5 mL water
ANALYSIS RECOMMENDATIONS
SAMPLE LOADING HPLC
Load 500 mL water sample
Elute at 5 mL/minute RECOMMENDED COLUMN

COLUMN WASHING Part No. N9303600

5 mL water
RELATED ITEMS
1 mL methanol
Vacuum Manifold -12 Position;; Part No. N9306619
DRYING Vacuum Manifold -24 Position;; Part No. N9306626
Vacuum Pump 20 L/min 115V, Part No. N9308035

12

ENVIRONMENTAL
2,4-Dichlorophenoxyacetic Acid in Water

Adjust the pH of 500 mL of water to 1.5 to 2 using 0.5 M H2SO4
packing
COLUMN CONDITIONING
3 mL of tetrahydrofuran
5 mL of methanol Let methanol infiltrate the packing material for 2 minutes

SAMPLE LOADING Collect the eluate and reconstitute to 3 mL usingmobile phase
Load the 500 mL sample at a rate no greater than 5 mL/min
RELATED ITEMS
COLUMN WASHING
DRYING

pressure manifold)


ENVIRONMENTAL
4'4-Methylenedianaline in Serum
PerkinElmer SPE Supra-Clean C18-S 100 mg/1 mL, Plastic Tube (Straight) Part No. N9306478

COLUMN CONDITIONING ANALYSIS RECOMMENDATIONS
3 mL of methanol Inject 10 µμL onto HPLC system
Extracted 100 µμg/mL sample
Mobile phase: methanol/water (50:50)
SAMPLE LOADING
Injection volume: 10 µμL
Load sample at 1 mL/minute

COLUMN WASHING RECOMMENDED COLUMN

Part No. N9303561
ELUTION
0.25 mL of methanol containing 1 M ammonium hydroxide RELATED ITEMS

14

ENVIRONMENTAL
Acephate in Water

SAMPLE PRETREATMENT CONCENTRATION
Prepare a 10 mL, 10 ppm sample of acephate in ammonium Evaporate to full dryness under a stream of nitrogen
sulphate aqueous solution (w/w 20%) Reconstitute the sample to 0.5 mL with water

2 mL of methanol Mobile phase: ACN/water (40:60, v/v)

Temperature: 30°C
SAMPLE LOADING
Load 4 mL samples at 1 to 2 mL/minute
RECOMMENDED COLUMN


RELATED ITEMS
ELUTION Vacuum Manifold -12 position;; Part No. N9306619
5 mL of methanol Vacuum Manifold -24 position;; Part No. N9306626


ENVIRONMENTAL
Aniline in Solution

Evaporate to full dryness at room temperature under a stream of
20 and 2 ppm nitrogen
Reconstitute the sample to 1 mL with methanol
COLUMN CONDITIONING
3 mL of methanol
Mobile phase: methanol/water (50:50, v/v)

SAMPLE LOADING RECOMMENDED COLUMN
Load 3 mL sample at 1 to 2 mL/minute
250 mm x 4.6 mm x 5 um Part No. N9303549

COLUMN WASHING RELATED ITEMS
Vacuum Manifold -12 position;; Part No. N9306619
Vacuum Manifold -24 position;; Part No. N9306626
ELUTION Vacuum Pump 20 L/min 115V, Part No. N9308035
3 mL of methanol/water (95:5, v/v) Vacuum Pump 17 L/min 230V, Part No. N9308331

16

ENVIRONMENTAL
Atrazine in Water

To 10 mL of water containing 10 ppm atrazine, add 20 µμL of Evaporate to full dryness under a stream of nitrogen
acetic acid Reconstitute the sample to 0.5 mL with water

2 mL of methanol Mobile phase: ACN/0.2% acetic acid (10:90, v/v)

Temperature: 30°C
SAMPLE LOADING
RECOMMENDED COLUMN

COLUMN WASHING
Part No. N9303561

RELATED ITEMS
ELUTION
5 mL of methanol Vacuum Manifold -24 Position;; Part No. N9306626


ENVIRONMENTAL
Bentazone in Water

Adjust the pH of 500 mL of water to 3 using 0.5 M H2SO4
the XC packing
COLUMN CONDITIONING
3 mL of tetrahydrofuran
5 mL of methanol Wait for 2 minutes to make sure the methanol infiltrates
the packing material

Elute the column with 3 mL of tetrahydrofuran
SAMPLE LOADING
Load the 500 mL sample at a rate no greater than 5 mL/min Evaporate the tetrahydrofuran and reconstitute to 3 mL using
mobile phase

COLUMN WASHING RELATED ITEMS
DRYING Vacuum Pump 20 L/min 115V, Part No. N9308035
pressure manifold)

18

ENVIRONMENTAL
Bentazone in Water, Derivitized

SAMPLE PRETREATMENT DRYING
Adjust the pH of 500 mL of water to 3 using 0.5 M H2SO4

COLUMN CONDITIONING ELUTION
3 mL of tetrahydrofuran 3 mL tetrahydrofuran
5 mL of methanol Concentrate sample to 3 mL under N2

RELATED ITEMS
SAMPLE LOADING Vacuum Manifold -12 Position;; Part No. N9306619
Load the 500 mL sample at a rate no greater than 5 mL/min Vacuum Manifold -24 Position;; Part No. N9306626
COLUMN WASHING


ENVIRONMENTAL
Chlorophenol in Water

Collect 500 mL of water Concentrate sample to 3 mL under nitrogen
Adjust pH to 2 with H2SO4
COLUMN CONDITIONING HPLC
5 mL methanol
5 mL water RECOMMENDED COLUMN

SAMPLE LOADING Part No. N9303600
Load 500 mL water sample
Elute at 5 mL/minute RELATED ITEMS
COLUMN WASHING Vacuum Manifold -24 Position;; Part No. N9306626
5 mL water
1 mL methanol

ELUTION
3 mL tetrahydrofuran

20

ENVIRONMENTAL
Chlorophenoxy Acid Herbicides in Water
PerkinElmer SPE Supra-Clean C18 1 g /6 ml, Plastic Tube (Straight) Part No. N9306422

Adjust pH of 1 L of water sample to pH 1.0 with hydrochloric acid 10 mL of hexane/acetone (50:50)

COLUMN CONDITIONING CONCENTRATION
10 mL of hexane/acetone (50:50)
10 mL of acidified methanol (5% HCl in methanol) Evaporate to 500 µμL under a nitrogen stream at room temperature

SAMPLE LOADING Inject 1 to 2 µμL onto GC
Load 1 liter of sample at a rate of 8 to 10 mL/minute
RELATED ITEMS
DRYING


ENVIRONMENTAL
N,N-Dimethylaniline in Solution

Evaporate to full dryness at room temperature under a stream
concentrations of 200, 20 and 2 ppm of nitrogen
Reconstitute the sample to 1 mL with methanol
COLUMN CONDITIONING
3 mL of methanol
Mobile phase: methanol/water (50:50, v/v)

Load 3 mL sample at 1 to 2 mL/minute
COLUMN WASHING
RELATED ITEMS
ELUTION
3 mL of methanol/water (95:5, v/v) Vacuum Pump 17 L/min 230V, Part No. N9308331

22

ENVIRONMENTAL
Nitroanalines in Solution

Prepare solutions of 2-nitroaniline and 4-nitroaniline in 0.1% Evaporate to full dryness at room temperature under a stream
ammonia aqueous at concentrations of 20, 2 and 0.2 ppm of nitrogen

COLUMN CONDITIONING Reconstitute the sample to 1 mL with methanol
3 mL of methanol
Mobile phase: methanol/1% formic acid (10:90, v/v)
SAMPLE LOADING
RECOMMENDED COLUMN

COLUMN WASHING
1 mL of 0.1% ammonia aqueous solution RELATED ITEMS
ELUTION Vacuum Manifold -24 Position;; Part No. N9306626
3 mL of methanol/1% formic acid (95:5, v/v) Vacuum Pump 20 L/min 115V, Part No. N9308035


ENVIRONMENTAL
Nitrobenzene in Water

Ensure that a 497.5 mL sample of water is pH neutral
packing
To this sample, add 2.5 mL of methanol

COLUMN CONDITIONING
3 mL of hexane Wait for 2 minutes to make sure the acetone infiltrates
5 mL of methanol the packing material

Connect the Supra-Poly XC column to a column packed with 5 g of
SAMPLE LOADING anhydrous sodium sulphate which has been washed with 3 mL of
acetone, 3 mL of hexane and 3 mL acetone
Load the 500 mL sample at a rate no greater than 5 mL/min

Elute the column series with 10 mL of hexane/acetone
COLUMN WASHING (90:10, v/v)

Collect the eluate and concentrate to 1 mL with nitrogen at 40 °C

DRYING RELATED ITEMS
pressure manifold) Vacuum Manifold -24 Position;; Part No. N9306626

24

ENVIRONMENTAL
Nitrobenzene in Water

Add methanol to water sample to provide a 0.5% solution
Adjust pH to 7
ELUTION
COLUMN CONDITIONING 10 mL n-hexane/acetone (90:10, V/V)
3 mL n-hexane Concentrate sample to 1 mL
5 mL methanol
RECOMMENDED COLUMN
SAMPLE LOADING
Load 10 mL water sample Part No. N9303561
Elute at 5 mL/minute
RELATED ITEMS


FORENSIC
6-Acetylmorphine in Urine
PerkinElmer SPE Supra-Clean Mixed-Mode MM1 200 mg/15 ml, Plastic Tube (Straight) Part No. N9306713

To 2 mL of 100 mM phosphate buffer (pH= 6.0) add internal 3 mL CH2Cl2/IPA/NH4OH (78:20:2) at a flow rate of 1-2 mL/min
standard*

Mix/vortex CONCENTRATION
Evaporate to dryness at < 40 °C
Add 4 mL of urine

Centrifuge for 10 minutes at 2,000 rpm POST TREATMENT
Add 50 µμL ethyl acetate
Mix/vortex

Adjust pH to 6 with 100 mM monobasic or dibasic sodium
Overlay with N2 and cap
phosphate
Mix/vortex
React 45 minutes at 70 °C;; cool.
* Suggested internal standard D6-6-AM-TMS

COLUMN CONDITIONING
Inject 2 µμl to a GC/MS
3 mL methanol

RESULTS
1 mL 100 mM phosphate buffer (pH 6) Ions to monitor (Mass Spectrometry)

Compound Primary Ion Secondary Tertiary
SAMPLE LOADING D6-6-AM-TMS 405 406 343
6-AM-TMS 399 400 340
Load the previously prepared sample onto the SPE column at a
flow rate of 1 mL/min
RECOMMENDED COLUMN
COLUMN WASHING
PerkinElmer Elite-5 MS 30 m x 0.25 mm x 0.25 um
Part No. N9316282
2 mL 100 mM acetate buffer (pH 4.5)
3 mL methanol RELATED ITEMS
DRYING

26

FORENSIC

PerkinElmer SPE Supra-Clean Mixed-Mode MM1 200mg/15ml, Plastic Tube (Straight) Part No. N9306713

To 2 mL of urine add internal standard(s)*, 1 mL of 100 mM
phosphate buffer (pH 6.0) and 1 mL of 0.35 M sodium periodate Evaporate to 30 µμL at < 40°C

Mix/vortex POST TREATMENT

Incubate at room temperature for 20 minutes
Overlay with N2 and cap
Adjust pH to 6.0±0.5 with 100 mM monobasic or dibasic sodium
phosphate React for 20 minutes at 70 °C
* Suggested internal standards D5-amphetamine and
D5-methamphetamine ANALYSIS RECOMMENDATIONS
Inject 2 µμl to a GC/MS
COLUMN CONDITIONING
3 mL methanol RESULTS
Ions to monitor (Mass Spectrometry)
1 mL 100 mM phosphate buffer (pH 6)
SAMPLE LOADING D5-amphetamine 194 92 123
Amphetamine 190 91 118
Load the previously prepared sample onto the SPE column at a D5-methamphetamine 208 92 163
flow rate of 1-2 mL/min Methamphetamine 204 91 160

COLUMN WASHING
RECOMMENDED COLUMN
1 mL 100 mM acetic acid PerkinElmer Elite-5 MS 30 m x 0.25 mm x 0.25 um
3 mL methanol Part No. N9316282

3 mL CH2Cl2/IPA/NH4OH (78:20:2) at a flow rate of 1-2 mL/min Vacuum Pump 17 L/min 230V, Part No. N9308331


FORENSIC
Anabolic Steroids in Urine

ß-Glucuronidase hydrolysis: To 5 mL of urine add suitable internal Evaporate to dryness at < 40 °C
standards and 2 mL of ß-Glucuronidase
ß POST TREATMENT
acetate buffer (pH 5.0)
(with 3% trimethylsilyliodide)
Mix/vortex Overlay with N2 and cap
Mix/vortex
Hydrolyze for 3 hours at 65 °C;; cool. React for 20 minutes at 70 °C
Remove from heat source to cool
Centrifuge for 10 minutes at 2,000 rpm and discard pellet
Adjust sample pH to 6.0±0.5 with approximately 700 µμL of 1.0 N
NaOH Inject 2 µμl to a GC/MS

COLUMN CONDITIONING RESULTS

3 mL methanol then aspirate Ions to monitor (Mass Spectrometry)
Compound Primary Ion Secondary Tertiary Other
1 mL 100 mM phosphate buffer (pH 6) then aspirate Testosterone-TMS 432 301 209
19-noretiocholanone-TMS 405 315 225
Oxymethalone 640 52 462 370, 143
SAMPLE LOADING Dehydroepiandosteronw-2TMS 432 327 297
Load the previously prepared sample onto the SPE column at 10-nortestosterone-2TMS 418 287 194
1-2 mL/min flow rate Oxymethalone metabolite #1 640 52 462 143
Oxymethalone metabolite #2 625 462 370 143
11-ß-hydroxyandosterone 522 417 158
COLUMN WASHING
Methandienone 409 313 281
19-norandosterone-2TMS 405 315 225
Alpha-hydroxyetiocholanone 504 417
1 mL hexane or hexane/ethyl acetate (50:50) 17-a-epitestosterone-TMS 432 341 327 209
Stanazolol 472 381 342 149

DRYING
RECOMMENDED COLUMN
ELUTION Part No. N9316279

Option 1: Elute with 3 mL of CH2Cl2/IPA/NH4OH (78:20:2) at
RELATED ITEMS
1-2 mL/min
Option 2: 3 mL CH2Cl2/IPA (80:20) Vacuum Manifold -12 Position;; Part No. N9306619
Option 3: 3 mL ethyl acetate Vacuum Manifold -24 Position;; Part No. N9306626
Option 4: 3 mL methanol Vacuum Pump 20 L/min 115V, Part No. N9308035

28

FORENSIC
Antidepressants/Painkillers in Urine and Blood

To 1 mL of 100 mM phosphate buffer (pH 6.0) add internal Evaporate to dryness at < 40 °C
standard*
POST TREATMENT
Add 1 mL of urine or blood
Reconstitute sample in 100 µμL of methanol
Add 2 mL of 100 mM phosphate buffer (pH 6.0)
Mix/vortex
Inject 2 µμl onto a LC

Adjust pH 6.0±0.5 with 100 mM of monobasic or dibasic sodium
phosphate RESULTS
Mix/vortex
Compound Detection Ions
Centrifuge Amitriptyline 278.8 / 91.1
Amitriptyline-D3 281.2 / 91.2

* Suggested internal standards Amitriptyline-D3, Diphenhydramine 256.2 / 167.1
Diphenhydramine-D3 259.2 / 167.1
Diphenhydramine-D3, Methadone-D9, Norpropoxyphene-D5, Doxepin 280.2 / 107.1
Propoxyphene-D11, Tramadol-D3 EDDP 278.2 / 234.2
EDDP-D3 281.4 / 234.3
COLUMN CONDITIONING Methadone 310.2 / 105.1
Methadone-D9 319.2 / 268.3
3 mL methanol Nortriptyline 264.2 / 91.1
Norpropoxyphene 326.2 / 44.1
1 mL 100 mM phosphate buffer (pH 6) Norpropoxyphene-D5 331.1 / 267.1
Propoxyphene 340.2 / 58.1
SAMPLE LOADING Propoxyphene-D11 351.3 / 64.0
Sertraline 308.1 / 161.0
Load the previously prepared sample onto the SPE column at Tramadol 264.2 / 58.1
1-2 mL/min Tramadol-D3 268.2 / 58.0
Venlafaxine 278.2 / 58.2
COLUMN WASHING Zolpidem 308.2 / 235

3 mL of 1% acetic acid RECOMMENDED COLUMN
3 mL methanol
Part No. N9303556
DRYING

RELATED ITEMS
Elute with 3 mL of ethyl acetate: acetonitrile: ammonia Vacuum Manifold -24 Position;; Part No. N9306626
(78:20:2, v/v/v) at 1-2m L/min Vacuum Pump 20 L/min 115V, Part No. N9308035


FORENSIC
Benzoylecgonine in Urine

SAMPLE PRETREATMENT
Benzoylecgonine 240 361 256
2 mL 100 mM phosphate buffer (pH 6) d3-benzoylecgonine 243 364

COLUMN CONDITIONING CHROMATOGRAM / SPECTRUM
3 mL methanol


SAMPLE LOADING
Load the previously prepared sample at 1-2 mL/min

COLUMN WASHING

100 mM HCL
1 mL of methanol

ELUTION
3 mL Methylene chloride:
Isopropanol:Ammonium Hydroxide (78:20:2) into conical tube

CONCENTRATION
Evaporate to dryness < 50 °C
RECOMMENDED COLUMN
POST TREATMENT PerkinElmer Elite-5 12 m x 0.20 mm x 0.33 µμm Part No. N9316110
Helium carrier – 2 mL/min

Cover with N2, cap, mix, heat to 70 °C and hold for 20 min. RELATED ITEMS
Evaporate to dryness < 50 °C. Vacuum Manifold -12 Position;; Part No. N9306619
Reconstitute in 100 µμL ethyl acetate Vacuum Manifold -24 Position;; Part No. N9306626
Transfer final treated sample to low volume autosampler vial insert Vacuum Pump 20 L/min 115V, Part No. N9308035
NOTES
Inject 1 µμL into GC/MS
Acetic Acid, 100 mM = 2.86 mL glacial acetic acid diluted to 500 mL
HPO4 +
RESULTS 2
12.14 g Na2HPO4
Three ion ratio chromatograms must all apex within ±2 scans with 100 mM Na2HPO4 (raises pH) or 100 mM Na2HPO4 (lowers pH).
of standard retention time. Ion ratios must fall within ±20% of Methylene Chloride/Isopropanol/Ammonium Hydroxide(78:20:2)
extraction solvent = 40 mL IP-OH + 4 mL concentrated NH4OH +
primary ion and only 1 confirmation ion. 156 mL MeCl2. Make fresh daily.

Compound Primary Ion Secondary Tertiary REFERENCES
Benzoylecgonine 300 421 316
d3-benzoylecgonine 303 424

30

FORENSIC
Carboxy-delta-9-THC, Delta-9-THC, Delta-9-Hydroxy THC in Whole Blood
PerkinElmer SPE Supra-Clean Mixed-Mode MM3 500 mg/6 mL, Plastic Tube (Straight) Part No. N9306649

Add internal standards* to 1 to 2 mlL of whole blood Evaporate to dryness < 40 °C

Mix/vortex
POST TREATMENT
Vortex and add dropwise 1 mL of cold acetronitrile

Centrifuge and transfer acetronitrile to a clean tube Mix/vortex

Adjust sample pH to 3.0±0.5 with approximately 2.0 mL of React for 20 minutes ot 70 °C
100 mM sodium acetate buffer
Cool
* Suggested internal standards D3-Carboxy-delta-9-THC;;
D3-delta-9-THC
Inject 1 to 2 µμL to a GC/MS
COLUMN CONDITIONING
RESULTS
5 mL methanol
2 mL acetate buffer (pH 3.0) then aspirate
SAMPLE LOADING D3-Carboxy-delta-9-THC 374 476 491
D9-Carboxy-delta-9-THC 380 479 497
Load sample at 1 to 2 mL/min Carboxy-delta-9-THC 371 473 488
D3-Hydroxy-delta-9-THC 374 462 477
Hydroxy-delta-9-THC 371 459 474
COLUMN WASHING D3-delta-9-THC 374 389
Delta-9-THC 371 386

4 mL 100 mM HCl/acetronitrile (95:5)

RECOMMENDED COLUMN
pressure manifold)
400 µμL hexane then aspirate PerkinElmer Elite-5 MS 15 m x 0.25 mm x 0.25 um
Part No. N9316279
DRYING
RELATED ITEMS
4 mL hexane
5 mL hexane/ethyl acetate (50:50)


FORENSIC
Delta-9-THC, Delta-9-Hydroxy THC, Carboxy-Delta-9-THC in Whole Blood

Add internal standards* to 1 to 2 mL of whole blood Evaporate to dryness with air or nitrogen at < 40 °C

Vortex and add dropwise 2 mL of cold acetronitrile
POST TREATMENT
Mix and centrifuge;; transfer acetronitrile to a clean tube Add 50 µμl of ethly acetate

Evaporate acetronitrile under air or nitrogen to 200 µμL Mix/vortex

)

* Suggested internal standards D3-Carboxy-delta-9-THC;; D3-delta-9- React for 20 minutes ot 70 °C
THC;; D3-Hydroxy-delta-9-THC
Cool

SAMPLE LOADING
Load sample directly onto column (no preconditioning)
Inject 1 to 2 µμL to a GC/MS

COLUMN WASHING RECOMMENDED COLUMN
hydroxide (84:15:1) Part No. N9316440

5 mL hexane/ethyl acetate/glacial Acetic acid (49:29:2) at a flow
rate of 1 to 2 mL/min

32

FORENSIC
Gamma-Hydroxybutyrate (GHB) in Blood, Urine, and Tissue

Pipet 200 µμL sample into 1.5 mL plastic tubes Evaporate to dryness at 70 °C under nitrogen

Add 25 µμL internal standard*
POST TREATMENT
Add 1 mL of acetone
Mix/vortex
Centrifuge
Heat at at 70 °C for 30 minutes
Transfer acetone layer to culture tube
Evaporate extract with nitrogen at 70 °C Inject 1 to 2 µμL to a GC/MS

Reconstitute extracts with 200 µμL of 100 mM phosphate buffer
RESULTS
(pH 6.0)
Mix/vortex
* Suggested internal standard D6-GHB GHB-D6-di-TMS 239 240 241
GHB-di-TMS 233 234 235
COLUMN CONDITIONING
5 mL methanol
RECOMMENDED COLUMN
2 mL 100 mM phosphate buffer (pH 6.0) Part No. N9316440

RELATED ITEMS
SAMPLE LOADING
Load the previously prepared sample onto the SPE column Vacuum Manifold -24 Position;; Part No. N9306626
2 mL methanol/ammonium hydroxide (99:1) in the original sample
test tube

Mix/vortex

Pour into column and collect extract


FORENSIC
Gamma-Hydroxybutyrate (GHB) in Urine without conversion to Gamma-Butrylactone (GBL)

SAMPLE PRETREATMENT CLEANUP
Pipet 200 µμL sample into a test tubes Add 200 µμL of dimethylformamide
Add 1 mL of hexane saturated with dimethylformamide
Add internal standard* and 100 µμL 100mM phosphate buffer Mix by inversion for 5 minutes
(pH 6.0) Centrifuge at 3000 rpm for 5 minutes.
Mix/vortex Transfer lower dimethylformamide layer to a clean test tube
Evaporate to dryness at < 50 °C under air or nitrogen
* Suggested internal standard D6-GHB
POST TREATMENT
COLUMN CONDITIONING
5 mL methanol

2 mL 100 mM phosphate buffer (pH 6.0) Inject 1 to 2 µμL onto a GC/MS

RESULTS
SAMPLE LOADING
Load the previously prepared sample onto the SPE column and
Sample load and wash are both collected GHB-D6-di-TMS 239 240 241
GHB-di-TMS 233 234 235

COLUMN WASHING
Add 2 mL methanol/sodium hydroxide (99:1) to the original s RECOMMENDED COLUMN
ample test
Mix/vortex thoroughly
Part No. N9316440

collected in previous step
RELATED ITEMS

Evaporate to dryness at 60 °C under air or nitrogen

34

FORENSIC
Opiates in Urine

SAMPLE PRETREATMENT CHROMATOGRAM / SPECTRUM

conc. HCl, vortex, heat 30 min at 120 °C

Cool, centrifuge, decant and keep top layer. Add 1 mL of 7.4 N
ammonium hydroxide, vortex. Adjust pH to 6.0 with 1-3 mL of
500 mM phosphoric acid

COLUMN CONDITIONING
3 mL methanol

1 mL 100 mM phosphate buffer (pH6)

SAMPLE LOADING
Load the prepared sample onto the SPE column at 1-2 mL/min

COLUMN WASHING

1 mL 100 mM acetic acid
RECOMMENDED COLUMN
1 mL of methanol
PerkinElmer Elite-5 12 m x 0.20 mm x 0.33 µμm Part No. N9316010
ELUTION Helium carrier – 2 mL/min.

3 mL Methylene chloride:Isopropanol:Ammonium Hydroxide
RELATED ITEMS
(78:20:2) into conical tube
CONCENTRATION
Evaporate to dryness < 50 °C Vacuum Pump 17 L/min 230V, Part No. N9308331

POST TREATMENT NOTES
Reconstitute and derivatize dried extract with 50 mL ethyl acetate, Acetic Acid, 100 mM = 2.86 mL glacial acetic acid diluted to 500 mL
2
HPO4 +
Cover with nitrogen, cap, mix, heat 70 °C (20 min), cool, do not 12.14 g Na2HPO4
evaporate with 100 mM Na2HPO4 (raises pH) or 100 mM Na2HPO4 (lowers
pH). Methylene hloride/Isopropanol/Ammonium Hydroxide (78:20:2)
ANALYSIS RECOMMENDATIONS extraction solvent = 40 mL IP-OH + 4 mL concentrated NH4OH +
Transfer final treated sample to low volume autosampler vial insert, 156 mL MeCl2. Make fresh daily.
inject 1 µμL into GC/MS
REFERENCES
RESULTS

Drug Primary Ion** Secondary Tertiary
Codeine 371 234 343
d3-Codeine 374 237
Morphine 429 287 324
d3-Morphine 432 290


FORENSIC
Sympathomimetic Amines in Urine

SAMPLE PRETREATMENT
Drug Primary Ion Secondary Tertiary
Amphetamine 118 240 91
Add 2 mL 100 mM phosphate buffer (pH 6) d5-amphetamine 244 123
d8-amphetamine 243 126
COLUMN CONDITIONING Methamphetamine 118 210 254
d5-methamphetamine 258 213
3 mL methanol d8-methamphetamine 261 213

SAMPLE LOADING Amphetamine 118 140 91
d5-amphetamine 144 123
Load previously prepared sample at 1 to 2 mL/min d8-amphetamine 143 126
Methamphetamine 154 118 110
COLUMN WASHING d5-methamphetamine 158 113

1ml of 100 mM acetic acid
1 mL of methanol CHROMATOGRAM

ELUTION
3 mL Methylene chloride:
Isopropanol:Ammonium Hydroxide (78:20:2) into conical tube

CONCENTRATION
Evaporate to dryness < 50 °C

POST TREATMENT

Cover with N2, cap, mix, heat 70 °C (20 min) Evaporate todryness RECOMMENDED COLUMN
< 50 °C. PerkinElmer Elite-5 12 m x 0.20 mm x 0.33 µμm Part No. N9316010
Reconstitute in 100 µμL ethyl acetate Helium carrier – 2 mL/min.

ANALYSIS RECOMMENDATIONS RELATED ITEMS
Transfer final treated sample to low volume autosampler vial insert, Vacuum Manifold -12 Position;; Part No. N9306619
inject 1 µμL into GC/MS Vacuum Manifold -24 Position;; Part No. N9306626
RESULTS Vacuum Pump 17 L/min 230V, Part No. N9308331

NOTES
Amphetamine 190 118 91 Acetic Acid, 100 mM = 2.86 mL glacial acetic acid diluted to 500 mL
d5-amphetamine 194 123 2
HPO4 +
d8-amphetamine 193 126 12.14 g Na2HPO4
Methamphetamine 204 160 118 with 100 mM Na2HPO4 (raises pH) or 100 mM Na2HPO4 (lowers
pH). Methylene hloride/Isopropanol/Ammonium Hydroxide(78:20:2)
extraction solvent = 40 mL IP-OH + 4 mL concentrated NH4OH +
156 mL MeCl2. Make fresh daily.

REFERENCES

36

PHARMACEUTICAL
Acetominophen in Serum

SAMPLE PRETREATMENT COLUMN WASHING

100 ppm solution
DRYING
Mix 25 mL of acetaminophen (100 ppm) solution in a 50 mL flask
and dilute to volume with water (standard solution 50 ppm)

Mix 25 mL of acetaminophen (100 ppm) solution in a 50 mL flask ELUTION
and dilute to volume with serum and 1% H3PO4 (sample 50% 2 mL of methanol
serum and 1% H3PO4)
CONCENTRATION
COLUMN CONDITIONING
Evaporate to dryness at < 50 °C using nitrogen
2 mL of methanol Reconstitute sample using 1 mL of mobile phase

RELATED ITEMS
SAMPLE LOADING
Load 2 mL of prepared sample Vacuum Manifold -24 Position;; Part No. N9306626


PHARMACEUTICAL
Acetominophen in Solution

Prepare a 5 ppm sample in 0.2% ammonium acetate Evaporate to full dryness under a stream of nitrogen
Reconstitute the sample to 1 mL with water
Adjust to pH 5

COLUMN CONDITIONING
PO4 (30:70, v/v)
2 mL of methanol 2

Temperature: 30 °C

SAMPLE LOADING
Load 4 mL samples at 1-2 mL/minute RECOMMENDED COLUMN

COLUMN WASHING
Part No. N9303561

RELATED ITEMS
ELUTION

38

PHARMACEUTICAL
Benzodiazepine Screen in Blood, Serum, and Tissue by GC/MS

To 1 ml of 100 mM phosphate buffer (pH=6) add internal Evaporate to dryness at < 40 °C under nitrogen
standards*
POST TREATMENT
Add 1 mL blood or 1 g of (1:4) tissue homogenate

Mix/vortex Heat at 70 °C for 30 minutes

Add 3 mL of 100 mM phosphate buffer (pH= 6) ANALYSIS RECOMMENDATIONS
Sample pH should be 6.0 ±0.5 (Adjust pH accordingly with 100 mM Inject 1 to 2 µμl to a GC/MS
monobasic or dibasic sodium phosphate)
RESULTS
Mix/vortex and centrifuge as appropriate
* Suggested internal standards Alprazolam-D,
Alphahydroxyalprazolam-D5, Diazepam-D5, Lorazepam-D4, Compound Primary Ion Secondary Tertiary
Alprazolam 308 279 204
Nordiazepam-D5, Oxazepam-D5, Temazepam-D5
Alprazolam-D** 513 284
Alphahydroxyalprazolam 318 396 383
COLUMN CONDITIONING Alphahydroxyalprazolam-D5 386 401
3 mL methanol Diazepam 256 283 284
Diazepam-D5** 287 289
3 mL 100 mM phosphate buffer 9pH 6)
Lorazepam 429 430 347
Lorazepam-D4** 433 435
SAMPLE LOADING Nordiazepam 34 342 343
Load previously prepared sample at 1 to 2 mL/min Nordiazepam-D5** 345 347
Oxazepam 429 313 430
Oxazepam-D5** 435 433
COLUMN WASHING Temazepam 343 257 283
Temazepam-D5** 348 262
3 mL of 5% (v/v) acetonitrile in 100 mM phosphate buffer (pH=6.0)
** Suggested internal standards
3 mL hexane RECOMMENDED COLUMN

DRYING PerkinElmer Elite-5 MS 30 m x 0.25 mm x 0.25 um
Part No. N9316282

RELATED ITEMS
ELUTION
3 mL ethyl acetate/ammonia (98:2 v/v) Vacuum Manifold -24 Position;; Part No. N9306626


PHARMACEUTICAL
Benzodiazepine Screen in Urine by GC/MS

Evaporate to dryness at < 40 °C under nitrogen
ß -Glucuronidase and add internal standards*
POST TREATMENT

Mix/vortex Heat at 70 °C for 30 minutes

Hydrolyze for 3 hours at 65 °C then cool ANALYSIS RECOMMENDATIONS
Centrifuge for 10 minutes at 2000 rpm and discard pellet Inject 1 to 2 µμl to a GC/MS

Add 3 mL of 100 mM phosphate buffer (pH 6.0) and mix RESULTS
* Suggested internal standards Alprazolam-D, Ions to monitor (Mass Spectrometry)
Alphahydroxyalprazolam-D5, Diazepam-D5, Lorazepam-D4,
Nordiazepam-D5, Oxazepam-D5, Temazepam-D5
Alprazolam 308 279 204
Alprazolam-D** 513 284
COLUMN CONDITIONING Alphahydroxyalprazolam 318 396 383
3 mL methanol Alphahydroxyalprazolam-D5 386 401
Diazepam 256 283 284
3 mL 100 mM phosphate buffer 9pH 6)
Diazepam-D5** 287 289
Lorazepam 429 430 347
SAMPLE LOADING Lorazepam-D4** 433 435
Load previously prepared sample at 1 to 2 mL/min Nordiazepam 34 342 343
Nordiazepam-D5** 345 347
Oxazepam 429 313 430
COLUMN WASHING Oxazepam-D5** 435 433
Temazepam 343 257 283
3 mL of 5% (v/v) acetonitrile in 100 mM phosphate buffer (pH=6.0)
Temazepam-D5** 348 262

3 mL hexane ** Suggested internal standards
RECOMMENDED COLUMN
DRYING
Part No. N9316282

ELUTION RELATED ITEMS
3 mL ethyl acetate/ammonia (98:2 v/v) Vacuum Manifold -12 Position;; Part No. N9306619

40

PHARMACEUTICAL
Beta Agonists in Urine

To 1 mL of 100 mM acetate buffer (pH 4.5) add 1 mL of urine Evaporate to dryness at < 40 °C

Add 2 mL of 100 mM Acetate buffer (pH 4.5) POST TREATMENT
Mix/vortex
5 mg/mL prepared in dry ethyl acetate (use molecular sieve). Store
Centrifuge this solution at –20 °C (freezer conditions) until use
Add 100 µμL of the methaneboronic acid solution to eluate
COLUMN CONDITIONING Mix/vortex
React 15 minutes at 70 °C;; cool
3 mL of methanol

3 mL 100 mM acetate buffer (pH 4.7)
Inject 1 to 2 µμl to a GC/MS
SAMPLE LOADING
RECOMMENDED COLUMN
Load the previously prepared sample onto the column at
1-2 mL/min PerkinElmer Elite-5 MS 30 m x 0.25 mm x 0.25 um
Part No. N9316282
COLUMN WASHING
RELATED ITEMS
2 x 1 mL acetone/methanol (1:1)
ELUTION
Elute with 1 mL dichloromethane/isopropanol/ammonium hydroxide
(78:20:2) at 1-2 mL/min


PHARMACEUTICAL
Beta Blockers in Blood and Urine

To 1 mL of 100 mM acetate buffer (pH 4.5) add 1 mL of blood or 1 mL dichloromethane/isopropanol/ammonium hydroxide (78:20:2)
urine

Add 2 mL of 100 mM Acetate buffer (pH 4.5) CONCENTRATION
Mix/vortex

Centrifuge POST TREATMENT

COLUMN CONDITIONING 5 mg/mL prepared in dry ethyl acetate (use molecular sieve). Store
this solution at –20 °C (freezer conditions) until use
3 mL of methanol Add 100 µμL of the methaneboronic acid solution to eluate
Mix/vortex
3 mL of 100 mM acetate buffer (pH 4.5) React 15 minutes at 70 °C;; cool

SAMPLE LOADING ANALYSIS RECOMMENDATIONS
Load the previously prepared sample onto the SPE column at Inject 1 to 2 µμl to a GC/MS
1-2 mL/min
RECOMMENDED COLUMN
COLUMN WASHING
2 x 1 mL acetone/methanol (1:1) Part No. N9316282


42

PHARMACEUTICAL
Caffeine, Theophylline and Theobromine in Blood, Plasma/Serum, and Urine

To 1 mL of 100 mM Acetic Acid add internal standard*

Add 1 ml blood, plasma/serum, or urine ELUTION
Add 2 mL of 100 mM Acetic Acid 3 mL ethyl acetate/methanol (90:10)

Mix/vortex
CONCENTRATION
Centrifuge Evaporate to dryness at < 40 °C
* Suggested internal standard 8-Chlorotheophylline
POST TREATMENT

COLUMN CONDITIONING Reconstitute sample in 1000 µμl of 0.1% formic acid (aq)

3 mL of methanol ANALYSIS RECOMMENDATIONS

1 mL of 100 mM acetic acid Inject 20 µμl on to an LC

SAMPLE LOADING RELATED ITEMS

Load the previously prepared sample onto the SPE column at Vacuum Manifold -12 Position;; Part No. N9306619
1-2 mL/min Vacuum Manifold -24 Position;; Part No. N9306626
COLUMN WASHING Vacuum Pump 17 L/min 230V, Part No. N9308331

3 mL 100 mM acetic acid


PHARMACEUTICAL
Cefaperazone in Water

SAMPLE PRETREATMENT ANALYSIS RECOMMENDATIONS
5 ppm of cefoperazone in water Mobile phase: 0.005 M tetrabutyl ammonium phosphate
(pH 3.63)/ACN (70:30, v/v)
COLUMN CONDITIONING
Temperature: 30 °C
2 mL of methanol

RECOMMENDED COLUMN
SAMPLE LOADING
5 um Part No. N9303549
COLUMN WASHING
RELATED ITEMS
ELUTION
6 mL of methanol Vacuum Pump 17 L/min 230V, Part No. N9308331

44

PHARMACEUTICAL
Clonazepam and 7-Aminoclonazepam in Urine

ß-Glucuronidase hydrolysis: To 2 mL of urine add internal standard Evaporate to dryness at <40 °C under nitrogen
and 1 mL ß-Glucuronidase solution*
POST TREATMENT

100 mM acetate buffer (pH 5.0)
Mix/vortex
Mix/vortex React 20 minutes 90°C;; cool

Hydrolyze for 3 hours at 65 °C;; cool ANALYSIS RECOMMENDATIONS
* Suggested internal standard Clonazepam-D4, Inject 1 to 2 µμl to a GC/MS
7-aminoclonazepam-D4
RESULTS
COLUMN CONDITIONING Ions to monitor (Mass Spectrometry)
3 mL methanol
3 mL water Clonazepam-TBDMS 372 374 326
Continue to condition with 1 ml 100 mM phosphate buffer (pH 6.0) 7-Aminoclonazepam-TBDMS 342 344 399
Clonazepam-D4-TBDMS 376 378 377
SAMPLE LOADING 7-Aminoclonazepam- 346 348 403
D4-TBDMS
Load the previously prepared sample onto the SPE column

RECOMMENDED COLUMN
COLUMN WASHING
Part No. N9316282
Wash the column with 2 mL 20% acetronitrile in 100 mM
phosphate buffer (pH 6.0)
RELATED ITEMS

2 mL hexane Vacuum Manifold -12 Position;; Part No. N9306619
Elute with 3 mL ethyl acetate with 2% ammonium hydroxide at
1-2 mL/min flow


PHARMACEUTICAL
DHEA, Testosterone, and Epitestosterone in Urine

To 5 mL of urine, add internal standard* and adjust sample pH to Add 5 mL of n-butyl chloride to sample. Cap the tube and shake
5.5-6.5 using concentrated sodium phosphate monobasic or dibasic vigorously for 10 minutes and then centrifuge at 3,000 rpm for 5
minutes. Transfer the organic layer to clean test tube and dry under
Mix a stream of nitrogen. Place dried sample in a desiccator and further
dry under Vacuum for 30 minutes.
Centrifuge samples at 3,000 rpm for 5 minutes

* Suggested internal standard at 20ng/mL: 16 a POST TREATMENT
Hydroxytestosterone
incubate at 70 °C for 20 minutes
COLUMN CONDITIONING Centrifuge at 3,000 rpm for 1 minutes and transfer to GC vial
3 mL methanol
1 mL 100 mM phosphate buffer (pH 6.0) Inject 1 to 2 µμl to a GC/MS

SAMPLE LOADING RESULTS
Load the previously prepared sample onto the SPE columnand allow Ions to monitor (Mass Spectrometry)
to flow via gravity
Cmopound Primary Ion Secondary
Testosterone 432 417
COLUMN WASHING Epitestosterone 432 417
DHEA 432 417
16 a Hydroxytestosterone 520 259

DRYING
RECOMMENDED COLUMN
PerkinElmer Elite-5 MS 30m x 0.25mm x 0.25um Part No. N9316282
ELUTION
3 mL methanol at 1-2 mL/min flow rate RELATED ITEMS
CLEANUP
Add 2 mL of 200 mM phosphate buffer (pH 7.0) and 250 units of Vacuum Pump 17 L/min 230V, Part No. N9308331
ß-glucuronidase
Mix/vortex and allow to incubate at 50 °C for 1 hour.
Cool sample, cap and adjust the pH to 10 to 11 using a 1:1 mixture
of NaHCO3/Na2CO3

46

PHARMACEUTICAL
Doxepin in Rat Serum

Mix 10 mL of doxepin aqueous solution (20mg/L) and 30 mL of rat Evaporate to full dryness at room temperature under a stream of
serum into a 100 mL vessel nitrogen
Reconstitute the sample to 1 mL with ACN:20 mM sodium acetate
(pH 4) (40:60, v/v)
solution
COLUMN CONDITIONING
Mobile phase: ACN:20 mM sodium acetate (pH 4) (40:60, v/v)
2 mL of methanol
Injection: 10 µμL
Temperature: 30 °C
SAMPLE LOADING
Load 2mL samples
RECOMMENDED COLUMN
COLUMN WASHING
2 mL of 0.5% ammonia solution containing 5% methanol Part No. N9303561

ELUTION RELATED ITEMS
2 mL of 1% acetic acid in methanol Vacuum Manifold -12 Position;; Part No. N9306619


PHARMACEUTICAL
Gabapentin in Blood, Plasma/Serum

To 500 µμL of 20% acetic acid add internal standard* Evaporate to dryness at < 40 °C

Mix thoroughly POST TREATMENT
Add 500 µμL of blood, plasma/serum

Mix thoroughly TCMS) and 50 µμL ethyl acetate
Cap and heat at 70 °C for 30 minutes
Centrifuge as appropriate Remove and allow to cool

COLUMN CONDITIONING
Inject 1 to 2 µμL onto GC/MS
3 mL of methanol

RECOMMENDED COLUMN
1 mL 100 mM HCl
PerkinElmer Elite-5MS 30 m x 0.25 mm x 0.25 µμm
SAMPLE LOADING Part No. N9316282
Load at 1 to 2 mL/minute
RELATED ITEMS
2
O
3 mL ethyl acetate
3 mL hexane

NOTES
DRYING
* Internal standard: 1-aminomethyl-1-cycloheptyl acetic

bis[Trimethylsilyl]trifluoroacetamide plus Trimethylchlorosilane
ELUTION
1 mL 2% ammonium hydroxide in methanol

48

PHARMACEUTICAL

To 0.2 to 0.5 mL of sample add 1 mL of acetone (dropwise) while
vortexing
ELUTION
Add internal standards*
3 mL methanol containing 2% ammonium hydroxide at 1-2 mL/min
Mix/Vortex and centrifuge flow rate

Transfer organic phase to ctean test tube and evaporate to dryness CONCENTRATION
Add 3 ml of 100 mM HCL Evaporate to dryness at < 40 °C

Mix/Vortex and centrifuge POST TREATMENT
* Suggested internal standards: Gabapentin-D10,
Aminocyclohexane-propionic acid
COLUMN CONDITIONING Inject 5 µμl on to an LC/MS
3 mL methanol
3 mL water RECOMMENDED COLUMN
1 mL 100mM HCl
Part No. N9303551
SAMPLE LOADING
Load the previously prepared sample onto the SPE column at RELATED ITEMS
1-2 mL/min Vacuum Manifold -12 Position;; Part No. N9306619
3 mL ethyl acetate
3 mL hexane


PHARMACEUTICAL

SAMPLE PRETREATMENT POST TREATMENT
Add internal standard to 500 mL of 20% Acetic acid and mix
thoroughly 50 µμL ethyl acetate
Cap and heat at 70 °C for 30 minutes
Add 500 µμL of blood, plasma/serum and mix thoroughly and Remove and allow to cool
centrifuge if necessary
COLUMN CONDITIONING
Transfer final treated sample to low volume autosampler vial insert,
3 mL methanol inject 1 -2 µμL into GC/MS

1 mL 100 mM HCl RECOMMENDED COLUMN

SAMPLE LOADING PerkinElmer Elite-5MS 30 m x 0.25 mm x 0.25 µμm
Part No. N9316282
RELATED ITEMS
3 mL ethyl acetate Vacuum Pump 20 L/min 115V, Part No. N9308035
3 mL hexane Vacuum Pump 17 L/min 230V, Part No. N9308331

NOTES
ELUTION
1 mL 2% ammonium hydroxide in methanol
trifluoroacetamide plus Trimethylchlorosilane.
CONCENTRATION
Evaporate to dryness at < 40°C

50

PHARMACEUTICAL
Ketotifen Fumarate in Solution

2mL of methanol
aqueous solution
POST TREATMENT
COLUMN CONDITIONING Evaporate to full dryness at room temperature under a stream of
nitrogen
2 mL of methanol
Reconstitute sample in methanol for analysis

RELATED ITEMS
SAMPLE LOADING
Load 2mL sample
COLUMN WASHING


PHARMACEUTICAL
Lovastatin in Water

Sample 1: 2 ppm lovastatin in 10% acetonitrile aqueous solution Evaporate to full dryness under a stream of nitrogen
Reconstitute the sample to 1 mL with methanol:1% formic acid
Sample 2: 0.2 ppm lovastatin in 1% acetonitrile aqueous solution solution (85:15, v/v)

2 mL of methanol Mobile phase: methanol:1% formic acid solution (85:15, v/v)

Temperature: 30 °C
SAMPLE LOADING
RECOMMENDED COLUMN
COLUMN WASHING

RELATED ITEMS
ELUTION
4 mL of acetonitrile

52

PHARMACEUTICAL
Methylmalonic Acid from Serum/Plasma


acetonitrile to 1 mL of sample
POST TREATMENT
Mix thoroughly

Centrifuge for 5 minutes at 2,000 rpm 25 µμL ethyl acetate
Heat for 20 minutes at 60 °C
COLUMN CONDITIONING
3 mL methanol
Transfer final treated sample to low volume autosampler vial insert,
inject 1 -2 µμL into GC/MS
SAMPLE LOADING
RECOMMENDED COLUMN
PerkinElmer Elite-5MS 30 m x 0.25 mm x 0.2 5 µμm

RELATED ITEMS
5 mL of methanol
DRYING Vacuum Pump 20 L/min 115V, Part No. N9308035

NOTES
ELUTION


PHARMACEUTICAL
Olanzapine in Whole Blood
PerkinElmer SPE Supra-Clean Cyano 500 mg/3 mL, Plastic Tube (Straight) Part No. N9306645

5 mL 1% acetic acid in methanol at 1 to 2 mL/min
Repeat the previous elution step
Add 1 ml blood

CONCENTRATION

Mix/vortex and centrifuge Evaporate to dryness at < 40 °C

*Suggested internal standard Prazepam POST TREATMENT
Reconstitute sample in 100 µμL 0.1% aqueous trifluoroacetic acid
COLUMN CONDITIONING
5 mL of methanol
Inject 50 µμL into HPLC

Part No. N9303624
COLUMN WASHING
RELATED ITEMS
5 mL of 1% acetic acid in water

54

PHARMACEUTICAL
Paroxetine in Blood, Plasma/Serum and Urine

To 1 mL of 100 mM phosphate buffer (pH= 6) add internal Evaporate to dryness at <40 °C under nitrogen
standards*
POST TREATMENT
Add 1 mL whole blood, serum/plasma or urine

Add 2 mL of 100 mM phosphate buffer (pH= 6)
Mix/vortex and centrifuge as appropriate
Inject 5 µμL onto LC/MS
* Suggested internal standard: Paroxetine-D6
RESULTS
COLUMN CONDITIONING
3 mL methanol Drug MRM Transition
3 mL water Paroxetine 330.0/190.1
3 mL 100 mM phosphate buffer (pH 6) Paroxetine-D6 336.0/76.1

SAMPLE LOADING
RECOMMENDED COLUMN
Load the previously prepared sample onto the SPE column

Part No. N9303565
COLUMN WASHING

3 mL 100 mM acetic acid RELATED ITEMS
3 mL methanol Vacuum Manifold -12 Position;; Part No. N9306619
3 mL ethyl acetate:acetonitrile:ammonium hydroxide (78:20:2) at a Vacuum Pump 17 L/min 230V, Part No. N9308331
flow rate of 1-2 mL/min


PHARMACEUTICAL
Propranolol in Rat Serum

Mix 10 mL of Propranolol aqueous solution (100 mg/L) and 30mL Evaporate to full dryness at room temperature under a stream of
of rat serum in to a 100 mL vessel nitrogen
Reconstitute the sample to 1 mL with ACN:20 mM sodium acetate
(pH 4) (30:70, v/v)
solution
COLUMN CONDITIONING Mobile phase: ACN:20 mM sodium acetate (pH 4) (40:60, v/v)
2 mL of methanol
Injection: 10 µμL
Temperature: 30 °C
SAMPLE LOADING
Load 2mL samples
RECOMMENDED COLUMN
COLUMN WASHING
2 mL of 0.5% ammonia solution containing 5% methanol

RELATED ITEMS
ELUTION
2 mL of 1% acetic acid in methanol

56

PHARMACEUTICAL
Tacrolimus, Cyclosporin and Rapamycin in Whole Blood

Add 50 mL whole blood and 50mL of 0.1 M ZnSO4 to a centrifuge
tube
ELUTION
Thoroughly mix
Add 750 mL of ethyl acetate
Add 500 mL methanol and internal standards* Collect eluate at 1 to 2 mL/minute
Thoroughly mix

Centrifuge for 2 min at 2000 rpm RECOMMENDED COLUMN

O
2 Part No. N9303508
Thoroughly mix
RELATED ITEMS
COLUMN CONDITIONING Vacuum Manifold -12 Position;; Part No. N9306619
SAMPLE LOADING
NOTES


COLUMN WASHING


PHARMACEUTICAL
Tricyclic Antidepressants in Plasma/Serum

To 2 mL of 100 mM phosphate buffer (pH= 6.0) add internal
standard*
ELUTION
Add 1 mL of plasma/serum
3 mL CH2Cl2/IPA/NH4OH (78:20:2) at 1 mL/min or gravity flow
Mix/vortex
CONCENTRATION
Centrifuge for 10 minutes at 2,000 rpm and discard pellet
Adjust pH to 6.0±0.5 with 100 mM monobasic or dibasic sodium
phosphate POST TREATMENT

* Suggested internal standards: Trimipramine, Protriptyline 2
O (1:3)
Mix/vortex
COLUMN CONDITIONING
3 mL methanol
3 mL water Inject 100 µμL onto HPLC
3 mL 100 mM phosphate buffer (pH=6)
RELATED ITEMS
SAMPLE LOADING Vacuum Manifold -12 Position;; Part No. N9306619
Load at 1 mL/min flow rate Vacuum Manifold -24 Position;; Part No. N9306626

1 mL of 100 mM acetic acid
3 mL methanol

58

ORDERING INFORMATION
Supra-Clean Columns and 96 Well Plates

PerkinElmer offers a comprehensive selection of SPE products that have been precisely manufactured for guaranteed reproducibility.

times. Supra-Clean and Supra-Poly SPE products are availabe in a range of media weights, volumes and bundles, including easy to
order selection kits and application packs.

SUPRA-CLEAN COLUMNS AND 96 WELL PLATES

Supra-Clean C18 Supra-Clean REC18
Supra-Clean C18 Columns Supra-Clean REC18 Columns

Media Weight Volume Part No. Quantity Media Weight Volume Part No. Quantity
50 mg 1 ml N9306476 50 50 mg 1 ml N9306519 50
100 mg 1 ml N9306478 100 100 mg 1 ml N9306520 100
100 mg 3 ml N9306523 50 100 mg 3 ml N9306455 50
200 mg 3 ml N9306462 50 200 mg 3 ml N9306521 50

500 mg 3 ml N9306438 50 500 mg 3 ml N9306522 50

500 mg 3 ml* N9306642 50 200 mg 6 ml N9306633 30

200 mg 6 ml N9306634 30 500 mg 6 ml N9306457 30

500 mg 6 ml N9306448 30 1 g 6 ml N9306491 30

500 mg 6 ml* N9306640 30 Supra-Clean REC18 96 Well Plates
1 g 6 ml N9306422 30
Media Weight Volume Part No. Quantity
2 g 6 ml N9306430 30
25 mg 2 ml N9306563 1
2 g 15 ml N9306479 20
50 mg 2 ml N9306564 1
2 g 25 ml N9306475 20
100 mg 2 ml N9306565 1
* Not end-capped

Supra-Clean C18 96 Well Plates Supra-Clean 300Å C4

Media Weight Volume Part No. Quantity Supra-Clean 300Å C4 Columns

25 mg 2 ml N9306566 1 Media Weight Volume Part No. Quantity
50 mg 2 ml N9306567 1 50 mg 1 ml N9306590 50
100 mg 2 ml N9306568 1 100 mg 1 ml N9306591 100
100 mg 3 ml N9306592 50
Supra-Clean C18 Cartridges
200 mg 3 ml N9306593 50
390 mg -- N9306587 50
Supra-Clean Strong Anion Exchange (SAX)
910 mg -- N9306588 50
Supra-Clean Strong Anion Exchange (SAX) Columns
1690 mg -- N9306589 50
50 mg 1 ml N9306553 50
100 mg 1 ml N9306471 100
100 mg 3 ml N9306554 50
200 mg 3 ml N9306482 50
500 mg 3 ml N9306555 50
500 mg 6 ml N9306556 30



Supra-Clean Strong Anion Exchange (SAX) 96 Well Plates Supra-Clean Mixed-Mode (MM1) 96 Well Plates

25 mg 2 ml N9306581 1 25 mg 2 ml N9306578 1
50 mg 2 ml N9306582 1 50 mg 2 ml N9306579 1
100 mg 2 ml N9306583 1 100 mg 2 ml N9306580 1

Supra-Clean Strong Cation Exchange (SCX) Supra-Clean Mixed-Mode (MM2)
Supra-Clean Strong Cation Exchange (SCX) Columns Supra-Clean Mixed-Mode (MM2) Columns

50 mg 1 ml N9306536 50 50 mg 1 ml N9306548 50
100 mg 1 ml N9306432 100 100 mg 1 ml N9306549 100
100 mg 3 ml N9306537 50 100 mg 3 ml N9306550 50
200 mg 3 ml N9306538 50 200 mg 3 ml N9306551 50
500 mg 3 ml N9306539 50 500 mg 3 ml N9306411 50
500 mg 6 ml N9306540 30 500 mg 6 ml N9306552 30

Supra-Clean Strong Cation Exchange (SCX) 96 Well Plates
Supra-Clean Mixed-Mode (MM3) Columns
25 mg 2 ml N9306575 1

100 mg 2 ml N9306577 1 500 mg 6 ml N9306649 30

Supra-Clean Weak Cation Exchange (WCX) Supra-Clean Florisil (FL-S)
Supra-Clean Weak Cation Exchange (WCX) Columns Supra-Clean Florisil (FL-S) Columns


50 mg 1 ml N9306544 50 200 mg 3 ml N9306511 50
100 mg 1 ml N9306545 100 500 mg 3 ml N9306512 50

100 mg 3 ml N9306546 50 500 mg 6 ml N9306494 30

200 mg 3 ml N9306547 50 1 g 6 ml N9306413 30

500 mg 3 ml N9306420 50 2 g 6 ml N9306513 20

500 mg 6 ml N9306407 30 2 g 15 ml N9306514 20
2 g 25 ml N9306515 20

Supra-Clean Mixed-Mode (MM1) * Granular shape

Supra-Clean Mixed-Mode (MM1) Columns
Supra-Clean Florisil (FL-S) Pesticide Grade
Media Weight Volume Part No. Quantity Supra-Clean Florisil (FL-S) Pesticide Grade Columns
50 mg 1 ml N9306541 50
100 mg 1 ml N9306542 100
200 mg 3 ml N9306516 50
100 mg 3 ml N9306419 50
500 mg 3 ml N9306400 50
200 mg 3 ml N9306543 50
500 mg 6 ml N9306517 30
500 mg 3 ml N9306481 50
1 g 6 ml N9306436 30
500 mg 6 ml N9306416 30
2 g 6 ml N9306470 30
200 mg 15 ml N9306713 20
2 g 15 ml N9306443 20
2 g 25 ml N9306447 20

* Granular shape

60


Supra-Clean Silica (SI-S) Supra-Clean Polyamine (P6)
Supra-Clean Silica (SI-S) Columns Supra-Clean Polyamine (P6) Columns

100 mg 3 ml N9306532 50 500 mg 3 ml N9306518 50
200 mg 3 ml N9306444 50 500 mg 6 ml N9306434 30
500 mg 3 ml N9306402 50
500 mg 6 ml N9306466 30 Supra-Clean Phenyl (PH-S)
1 g 6 ml N9306404 30 Supra-Clean Phenyl (PH-S) Columns
2 g 6 ml N9306533 20
2 g 15 ml N9306534 20
50 mg 1 ml N9306401 50
2 g 25 ml N9306535 20
100 mg 1 ml N9306524 100
Supra-Clean Silica (SI-S) Cartridges 100 mg 3 ml N9306525 50
200 mg 3 ml N9306490 50
500 mg 3 ml N9306421 50
300 mg -- N9306584 50
700 mg -- N9306585 50 500 mg 6 ml N9306526 30

1300 mg -- N9306586 50 1 g 6 ml N9306527 30

Supra-Clean Phenyl (PH-S) 96 Well Plates
Supra-Clean Cyano (CN-S)
Supra-Clean Cyano (CN-S) Columns 25 mg 2 ml N9306569 1
Media Weight Volume Part No. Quantity 50 mg 2 ml N9306570 1
500 mg 3 ml N9306645 50 100 mg 2 ml N9306571 1
500 mg 6 ml N9306644 30
Supra-Clean LCC
Supra-Clean Amino (NH2-S) Supra-Clean LCC Columns
Supra-Clean Amino (NH2-S) Columns
Media Weight Volume Part No. Quantity 500 mg 3 ml N9306643 50
50 mg 1 ml N9306528 50 500 mg 6 ml N9306641 30
100 mg 1 ml N9306410 100
100 mg 3 ml N9306529 50
500 mg 3 ml N9306414 50
200 mg 6 ml N9306530 50
500 mg 6 ml N9306531 30

Supra-Clean Amino (NH2-S) 96 Well Plates

25 mg 2 ml N9306572 1
50 mg 2 ml N9306573 1
100 mg 2 ml N9306574 1


Supra-Poly HLB Columns and 96 Well Plates

SUPRA-POLY HLB COLUMNS AND 96 WELL PLATES

Supra-Poly HLB Media Weight Volume Part No. Quantity
Supra-Poly HLB 30 µμm Columns 200 mg 6 ml* N9306693 30
500 mg 6 ml N9306684 30
500 mg 15 ml N9306685 20
30 mg 1 ml N9306650 50
500 mg 6 ml* N9306694 30
50 mg 1 ml N9306655 50
1 g 15 ml N9306686 20
60 mg 1 ml N9306656 50
30 mg 15 ml** N9306688 50
100 mg 1 ml N9306657 50
60 mg 15 ml** N9306689 50
30 mg 3 ml N9306651 50
100 mg 15 ml** N9306690 50
60 mg 3 ml N9306658 50
200 mg 15 ml** N9306691 50
100 mg 3 ml N9306659 50
1 g 25 ml N9306687 20
200 mg 3 ml N9306660 50
500 mg 3 ml N9306661 30 * Glass columns ** LRC columns
100 mg 6 ml* N9306672 30
Supra-Poly HLB 30 µμm 96 Well Plates
150 mg 6 ml N9306662 30
200 mg 6 ml N9306663 30
30 mg 2 ml N9306698 1
200 mg 6 ml* N9306673 30
50 mg 2 ml N9306699 1
500 mg 6 ml* N9306674 30
60 mg 2 ml N9306700 1
500 mg 6 ml N9306664 30
500 mg 15 ml N9306665 20 Supra-Poly HLB 60 µμm 96 Well Plates
1 g 15 ml N9306666 20 Media Weight Volume Part No. Quantity
30 mg 15 ml** N9306668 50 30 mg 2 ml N9306695 1
60 mg 15 ml** N9306669 50 50 mg 2 ml N9306696 1
100 mg 15 ml** N9306670 50 60 mg 2 ml N9306697 1
200 mg 15 ml** N9306671 50
1 g 25 ml N9306667 20

Supra-Poly HLB 60 µμm Columns

30 mg 1 ml N9306652 50
50 mg 1 ml N9306675 50
60 mg 1 ml N9306676 50
100 mg 1 ml N9306677 50
30 mg 3 ml N9306653 50
60 mg 3 ml N9306678 50
100 mg 3 ml N9306679 50
200 mg 3 ml N9306680 50
500 mg 3 ml N9306681 30
100 mg 6 ml* N9306692 30
150 mg 6 ml N9306682 30
200 mg 6 ml N9306683 30

62

Supra-Poly Columns and 96 Well Plates

SUPRA-POLY COLUMNS AND 96 WELL PLATES

Supra-Poly Extreme Capacity 1500 m2/g (XC)

Supra-Poly Extreme Capacity 1500 m2/g (XC) Columns
Supra-Poly Environmental (AEV)
Supra-Poly AEV Columns
30 mg 1 ml N9306441 50

60 mg 1 ml N9306501 50 100 mg 3 ml N9306648 50

100 mg 1 ml N9306403 50
60 mg 3 ml N9306502 50 Supra-Poly Hydrophilic (ATH)
100 mg 3 ml N9306440 50 Supra-Poly ATH Columns
200 mg 3 ml N9306428 50
200 mg 6 ml N9306635 30
100 mg 3 ml N9306646 50
500 mg 6 ml N9306405 30
200 mg 3 ml N9306638 50
1 g 15 ml N9306503 20
200 mg 6 ml N9306636 30

Supra-Poly Extreme Capacity 1500 m2/g (XC) 96 Well Plates
Supra-Poly Lipophilic (ATL)
30 mg 2 ml N9306557 1 Supra-Poly ATL Columns

60 mg 2 ml N9306559 1 100 mg 3 ml N9306647 50
200 mg 3 ml N9306639 50
Supra-Poly Extra Wide Particle 1200 m2/g 200 mg 6 ml N9306637 30
(XWP)
Supra-Poly Extra Wide Particle 1200 m2/g (XWP) Columns

30 mg 1 ml N9306504 50
50 mg 1 ml N9306427 50
60 mg 1 ml N9306505 50
100 mg 1 ml N9306506 50
60 mg 3 ml N9306507 50
100 mg 3 ml N9306508 50
200 mg 3 ml N9306509 50
500 mg 6 ml N9306418 30
1 g 15 ml N9306510 20

Supra-Poly Extra Wide Particle 1200 m2/g (XWP)
96 Well Plates

30 mg 2 ml N9306560 1
50 mg 2 ml N9306561 1
60 mg 2 ml N9306562 1


SPE Kits and Packs

SPE SELECTION KITS
Selection kits enable quick column selection for development of reproducible and repeatable SPE methods.

SPE Selection Kits

Description Media Weight Volume Part No. Quantity
Pre-Concentration of Hydrophobic Compounds from Aqueous Matrix 200 mg 6 ml N9306594 50
200 mg 3 ml N9306595 50
Extraction of Hydrophobic Compounds from Aqueous Matrix 500 mg 6 ml N9306596 50
500 mg 3 ml N9306597 50
Pre-Concentration of Hydrophilic Compounds 500 mg 6 ml N9306598 30
500 mg 3 ml N9306599 30
Removal of Polar Compounds from Aqueous and Organic Matrix 500 mg 6 ml N9306600 30
500 mg 3 ml N9306601 30
Extraction of Acidic Basic and Neutral Compounds from Aqueous or Organic Matrix 100 mg 3 ml N9306602 50
Extraction of Carboxylic Acids and Strong Bases from Aqueous Matrix 500 mg 6 ml N9306603 40
Extraction of Weak Bases from Aqueous Matrix 500 mg 6 ml N9306604 30

SPE APPLICATION PACKS
Ideal for extraction of known entities from a variety of matrices, our packs are expertly tailored to meet your application needs and
are designed to support major EPA methods and applications.

SPE Application Packs

Description Media Weight Volume Part No. Quantity
Extraction of Basic Drugs from Biological Fluids 200 mg 3 ml N9306605 50
Extraction of Bisphenol A from Aqueous Matrix 1 g 6 ml N9306613 30
Extraction of Oil and Grease from Aqueous Matrix-EPA 1664 500 mg 3 ml N9306612 50
1 g 6 ml N9306611 30
Extraction of PAH from Soil and Oil 1.5 g 6 ml N9306609 30
Extraction of PAH from Soil and Oil (Glass Straight Column) 1.5 g 6 ml N9306610 30
Extraction of PAH from Water Containing Humic Acids 1.5 g 6 ml N9306608 30
Extraction of PAH from Water or Soil 4 g 6 ml N9306606 30
Extraction of PAH from Water or Soil (Glass Straight Column) 4 g 6 ml N9306607 30
Extraction of PCB from Oil 1 g 6 ml N9306617 30
1 g 3 ml N9306616 50
Extraction of Pesticides and Herbicides from Aqueous Matrix 500 mg 3 ml N9306614 50
Extraction of Steroids from Biological Fluids 500 mg 6 ml N9306615 30
Extraction of SVOC from Water-EPA 525 1 g 6 ml N9306618 30

64

SPE Vacuum Pumps, Manifolds and Accessories

SPE VACUUM PUMPS, MANIFOLDS AND ACCESSORIES
PerkinElmer SPE Vacuum Manifolds allow multiple samples to be processed simultaneously by conveniently holding SPE media
cartridges in place and allowing samples to pass through them. SPE Vacuum Manifolds are available to accommodate either 12 or
24 cartridges;; 1, 3, 6, 15, and 25 mL cartridges can be used with the manifolds. Manifolds are equipped with a vacuum port where
a standard laboratory vacuum pump can be connected. Vacuum pulls the sample through the stationary phase, metered by the
stopcocks, to control the speed of the extraction process and the sample flow over the media bed in the SPE cartridge. Waste and
wash solvents are discarded and analytes are collected in sample tubes below the manifold completing the extraction.

SPE Manifolds and Accessories

Description Part No. Quantity
Vacuum Manifold - 12 Position N9306619 1 each
Vacuum Manifold - 24 Position N9306626 1 each
Replacement Chamber (Glass) - 12 Position N9306620 1 each
Replacement Chamber (Glass) - 24 Position N9306627 1 each
Cover Gasket - 12 Position N9306621 1 each
Cover Gasket - 24 Position N9306628 1 each
Stopcocks - 12 Position N9306624 12 pack
Stopcocks - 24 Position N9306631 24 pack
Needles - Polypropylene - 12 Position N9306622 12 pack
Needles - Polypropylene - 24 Position N9306629 24 pack
Needles - Stainless Steel - 12 Position N9306623 12 pack
Needles - Stainless Steel - 24 Position N9306630 24 pack
Drying Attachment - 12 Position N9306625 1 each
Drying Attachment - 24 Position N9306632 1 each

Vacuum Pumps

Description Part No. Quantity
Vacuum Pump 20 L/min 115V N9308065 1 each


At PerkinElmer, we understand that sample preparation is one of the most critical steps in the analytical
process. Often accounting for 60% of your timetable, it has a fundamental impact on a wide range of
operational parameters. Any errors within this process undermine the quality of your data at all subsequent
stages of your analysis.
Solid Phase Extraction helps avoid The right accessories, consumables, methods and
potential errors in sample preparation,
reducing re-runs and dramatically application support are as integral to the success
increasing productivity. As one of the
most cost-effective and flexible tools of your laboratory as your instrumentation. That’s
within the laboratory environment,
SPE also provides efficient sample
why we invest heavily in testing and validating our
concentration and purification prior complete portfolio of solutions to ensure you receive
to many of today’s most popular
analytical techniques, including HPLC, accurate, repeatable results on time, every time.
LC/MS, GC and GC/MS.

that encompasses instruments, accessories, consumables, supplies, training and service. It’s a breadth of
capabilities that enables us to offer the ease and convenience of having a single supplier for all your needs at
every stage of your workflow. So you can benefit from greater responsiveness, superior reliability, and dramatic
cost savings.
Our OneSource Laboratory Services division even takes it
Couple SPE With Leading a step further. With more than 1,500 trained and
Instrumentation For Ultimate certified field service engineers and service personnel
Laboratory Efficiency around the world, OneSource offers the most
Clarus® 680/580/480 GC comprehensive portfolio of professional laboratory
services in the industry, including complete care programs
Clarus SQ 8 GC/MS
for virtually every technology and manufacturer.
Flexar™ SQ 300 MS
Flexar LC and UHPLC

PerkinElmer, Inc.
940 Winter Street
Waltham, MA 02451 USA
P: (800) 762-4000 or
(+1) 203-925-4602
www.perkinelmer.com

For a complete listing of our global offices, visit www.perkinelmer.com/ContactUs

Copyright ©2012, PerkinElmer, Inc. All rights reserved. PerkinElmer® is a registered trademark of PerkinElmer, Inc. All other trademarks are the property of their respective owners.

010097_01 Printed in USA

Supra-Clean® and Supra-Poly® Solid Phase Extraction (SPE) Application Notebook

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