Sample Prep for Chromatographic Analysis of Difficult Matrixes

Sample Prep for Chromatographic 

Analysis of Difficult Matrixes

2

Real World & Real Samples

0

2

4

6

Time (min)

Urine Sample without sample prep

0

2

4

6

Time (min)

Urine Sample with sample prep

3

Sources of Chromatographic Errors

4

Time Spend on Analytical Process

5

Sample Prep Innovations

•

Solid Phase Microextraction (SPME)

•

High specificity SPE

•

Dispersive SPE

•

Silver Ion SPE for FAMEs

•

Carbonaceous adsorbents

•

Flash chromatography

6

Solid Phase Microextraction (SPME)

• “Sample Prep Made Easy”
• Enrichment technique mainly for trace analysis 
• Developed in collaboration with Janusz Pawliszyn, Univ. of Waterloo
• Unique and proprietary to Supelco

Users are...

•

GC and GC-MS analysts (HPLC & LC-MS)

•

Analyzing compounds in gases, liquids or 

solids.

Interested in...

•

Sample enrichment

•

Solventless extraction

•

Using existing GC & HPLC systems

•

Economical sample prep

•

Reducing lab animal sacrifice

Users can expect...

•

Highly consistent, quantifiable results from 

low concentrations of analytes

Users are...

•

GC and GC-MS analysts (HPLC & LC-MS)

•

Analyzing compounds in gases, liquids or 

solids.

Interested in...

•

Sample enrichment

•

Solventless extraction

•

Using existing GC & HPLC systems

•

Economical sample prep

•

Reducing lab animal sacrifice

Users can expect...

•

Highly consistent, quantifiable results from 

low concentrations of analytes

7

6.00

7.00

8.00

9.00

10.00 11.00 12.00 13.00 14.00 15.00

1

2

3

4

5

1.  2-Isopropyl-3-methoxypyrazine (IPMP)
2.  2-Isobutyl-3-methoxypyrazine (IBMP)
3.  2- Methylisoborneol (MIB)
4.  2,4,6-Trichloroanisole (I.S. 8ppt)
5.  (±) Geosmin

1.  2-Isopropyl-3-methoxypyrazine (IPMP)
2.  2-Isobutyl-3-methoxypyrazine (IBMP)
3.  2- Methylisoborneol (MIB)
4.  2,4,6-Trichloroanisole (I.S. 8ppt)
5.  (±) Geosmin

Odor-Causing Compounds in Water at 

2 ppt (GC/MS)

Sensitive

8

Linearity of Odor-Causing Compounds from 

Water at ppt Levels (SPME-GC/MS)

0.0

1.0

2.0

3.0

4.0

5.0

6.0

7.0

8.0

9.0

0

2

4

6

8

10

12

part per trillion

IPMP r2=0.9900, yint=+0.015 
IBMP r2=0.9959, yint=+0.028
MIB r2=0.9983, yint=0.021
Geosmin r2=0.9988, yint= -0.071

Quantitative

9

SPME Overview

• Solvent-free extraction technique for 

nearly any sample or matrix

• Alternative to head-space GC and solid 

phase extraction (SPE) techniques

• Directly interfaced with GC analysis
• Non-destructive to sample 
• Reusable (100+ times)
• Inexpensive
• Fast

Manual SPME holder 

and inlet guide.

Assembled SPME 

fiber and holder 

with fiber immersed 

in a liquid sample.

10

The SPME Concept

Click here for animation

11

SPME Fiber Coating: The Business 

End
•An equilibrium is set up between analytes dissolved in the sample 

(solution or gas phase) and in the liquid coating on the fiber.

•The fiber coating consists of:

•

GC-type phases

•

Particles

Enlargement of 

the SPME fiber 

coating

12

Distribution Constant

•Concentration of analyte in stationary phase compared to 

concentration of analyte in solution:

K = ns/V1C2°

K = Distribution constant

ns = Moles of analyte in stationary phase

V1 = Volume of stationary phase

C2° = Final analyte concentration in water

13

Analyte 

Adsorbed

Silica Rod

Liquid Polymer

Aqueous 

Solution

Vial

Time

Adsorption Mechanism for SPME

14

Absorbent vs. Adsorbent Fibers

Absorbent-type fibers

(Film-type fibers)

Analytes are extracted by partitioning

•

Liquid phase

•

Retains by thickness of coating

Analytes do not compete for sites
Fibers can have high capacity  

Adsorbent-type fibers

(Particle-type fibers)

Physically traps or interacts with 

analytes

•

Porous particles

•

High surface area

Analytes may compete for sites
Fibers have limited capacity

15

Types of SPME Fiber Coatings

Coating

Type

Polarity

7 µm Polydimethylsiloxane (PDMS)

Absorbent

Nonpolar

30 µm PDMS

Absorbent

Nonpolar

100 µm PDMS

Absorbent

Nonpolar

85 µm Polyacrylate (PA)

Absorbent

Polar

60 µm PEG (Carbowax)

Absorbent

Polar

Coating

Type

Polarity

85 µm Carboxen-PDMS 

Adsorbent

Bipolar 

65 µm PDMS-DVB 

Adsorbent

Bipolar

55 µm/30 µm DVB/Carboxen-PDMS 

Adsorbent

Bipolar

15 µm Carbopack Z-PDMS 

Adsorbent

Bipolar

Particles – Adsorption:

Films – Absorption:

16

PDMS-DVB Fiber SEM

• Cross section of the PDMS-DVB fiber.  The center is a fused silica core, 

surrounded by a Stableflex core. The 3-5µm DVB particles are 

suspended in PDMS and layered over the cores.  275x magnification.

Photomicrograph of SPME fiber provided by Prof. Dan Armstrong, U. Texas Arlington

17

PDMS-Carboxen Fiber SEM

• 3000X magnification of the Carboxen PDMS coating.  The 3-5µm 

Carboxen-PDMS particles are suspended in PDMS.

Photomicrograph of SPME fiber provided by Prof. Dan Armstrong, U. Texas Arlington

18

97-0340

Carboxen™ Particle – Volume 

Contribution

Contribution of pore types to total 

Carboxen pore volume:

micropores (2-20Å) = 0.29 mL/g
mesopores (20-500Å) = 0.26 mL/g
macropores (>500Å) = 0.23 mL/g

Macropore

Mesopore

Micropore

19

Physical Properties of Divinylbenzene 

and Carboxen 1006

Surface Area

Porosity (mL/g)*

Material                  (m2/g)               macro meso    micro

Divinylbenzene

750

0.58

0.85

0.11

Carboxen™ 1006

720

0.23

0.26

0.29

*Macropore = >500Å

Mesopore = 20-500Å

Micropore = 2-20Å

20

Comparison of SPME Fibers for the 

Extraction of Small Hydrocarbons

Analyte

100µm PDMS

PDMS/DVB

Carboxen/PDMS

Ethane

0

0

750

Propane

0

0

20000

Butane

0

340

72100

Pentane

230

2150

108000

Hexane

460

9280

105000

(Analytes at 1 ppm in air,  extracted for 10 min.)

(Absolute area responses)

Absorbent

Adsorbent

21

Molecular Weight Range for SPME 

Fibers

0

150

300

450

Molecular Weight Range

7µm PDMS

30µm PDMS

100µm PDMS

DVB

DVB-Carboxen

Carboxen

22

Area Response vs. Fiber Type

Acenaphthene            

MW 154

Decachlorobiphenyl

MW 502

Chrysene

MW 228

1.E+07

7.E+06

9.E+06

5.E+03

2.E+06

1.E+06

0.0E+00

2.0E+06

4.0E+06

6.0E+06

8.0E+06

1.0E+07

1.2E+07

30µm PDMS

Polyacrylate

PDMS-DVB

Carboxen-PDMS

23

Effects of Fiber Polarity & Coating 

Thickness

• Fiber Polarity

•

Analyte selectivity

•

Better recovery of polar analytes

•

PEG 

•

Polyacrylate

• Coating Thickness

•

Analyte selectivity

•

Extraction time                           

•

Sample capacity

•

Desorption time and carryover

24

Effects of Phase Coating Thickness of 

PDMS on Analyte Recovery Relative to 

Chrysene*

Analyte

%Relative Recovery

100µm

30µm

7µm

Benzene

2

1

<1

Toluene

5

1

<1

Naphthalene

13

4

1

Phenanthrene

37

27

16

Anthracene

49

38

32

Pyrene

69

54

47

Benzo(a)anthracene

105

91

96

Chrysene

100

100

100

Benzo(a)pyrene

119

127

131

Indeno(1,2,3-cd)pyrene

61

140

148

Benzo(g,h,i)perylene

61

117

122

*Absolute response of chrysene set to 100%

25

Factors Affecting Extraction Recovery

•Salts and pH
•Headspace vs. direct extraction
•Inlet liner volume
•Stirring (sample) & agitation (fiber)

•

Increases precision

•

Reduces time to reach equilibrium

•

Must be consistent for all analyses

•

Required for analytes with high 

distribution constants

•

Sonication may increase temperature

26

Effects of Salt and pH

Salt usually increases analyte uptake
Use 25-30% NaCl to salt-out samples                                                     
Salt is not necessary for large non-polar analytes, such as PAHs 

and large hydrocarbons, and may reduce recovery 

Lower pH to extract acidic compounds
Raise pH to extract basic compounds
Beware of stability of analytes at different pH levels

27

No Salt

No Salt

Salt

Salt

Neutral

pH = 2

Neutral

pH = 2

Phenol

810

1003

6425

6150

Methylphenol

761

882

5485

7434

2-Nitrophenol

422

474

311

2315

2,4-Dimethylphenol

1344

1476

15000

20710

2,4-Dichlorophenol

5396

8138

19803

61664

2,4,5-Trichlorophenol

3115

11097

24270

96333

2,4-Dinitrophenol

0

11

765

1182

4-Nitrophenol

626

730

6536

11438

2,3,4,6-Tetrachlorophenol

3108

27683

33938

70440

2-Methyl-4,6-dinitrophenol

55

47

920

1685

Pentachlorophenol

2305

40582

22056

143905

The Effect of Salt and pH on Extraction of 

Phenols by SPME

28

Headspace vs. Direct Immersion

•Analytical 

considerations:

•

Volatility of sample

•

Extraction time 

concerns

•

Sample matrix

•

Selectivity of analytes

Liquid or solid sample

Liquid sample

Headspace

extraction

Direct immersion

extraction

29

0.75mm ID Inlet Liner

50ppb

Standard Splitless Liner, 

2mm ID 

50ppb

94-0040

Inlet Liner Volume: Comparison for 

Analysis of Gaseous VOCs by SPME

1

4

5

3

2

3

4

5

794-0050, 0051

Min

2

6

1

4

5

3

2

2

3

4

5

Min

6

1. Chlormethane   

2. Vinyl chloride   

3. Bromomethane

4. Chloroethane    

5. Freon 11          

30

SPME Automation

•Compatible with common GC 

autosamplers (Gerstel MPS, 

CTC Combi PAL, etc.)

•Improves reproducibility by 

automating important 

variables:

•

Heating

•

Agitation

•

Equilibration time

•

SPME automation video (~2 mins.)

31

794-0862

0

4

8

Min

12

1. Solvent

2. Internal standard

3. cis-Menthone

4. trans-Menthone

5. Menthol

1

3

4

5

2

SPME Fiber: 100µm PDMS

Sample: 4g peppermint cookie bar

Extraction: headspace, 1 min, 45°C

Desorption: 5 min at 250°C

Column: PTE™-5, 30m x 0.25mm ID, 

0.25µm film

Detector:FID, 250°C

Injector: Splitless (3 min), 250°C

Peppermint Oil in Chocolate Cookie Bar

32

Milk Sample Off-Flavors by SPME-GC/MS

98-0385

Chromatogram provided by Ray Marsili, Dean Foods 

Technical Center, Rockford, IL, USA.

G00507, 508

1

3

2

IS

4

6

10

15

20

Min

25

30

35

5

IS

1. Acetone

2. 2-Butanone

3. 3-Methylpentane

4. Pentanal

5. Dimethyldisulfide

6. Hexanal

IS. 4-Methyl-2-pentanone

Prior to Exposure to 

Sunlight

After 1-Hour Exposure to 

Sunlight

SPME Fiber: 75 µm PDMS/Carboxen

Sample: 3g of 2% milk + 10µL internal 

standard solution, (20µg/mL 4-methyl-2-

pentanone) (9mL GC vial)

Column: Supel-Q™ PLOT, 30m x 0.32mm ID

Det.: GC/MS ion trap, m/z = 33-300

33

Residual Solvents in Commercial Ibuprofen 

Brand “A”

Brand “B”

2

4

6

8

10

12

Time (min)

0.00E+00

2.00E+06

4.00E+06

3

1

2

4

7

8

9

12

5

2

4

6

8

10

12

Time (min)

0.00E+00

2.00E+06

4.00E+06

9

1

2

4

5

6

7

8

10 11

12

1.

Acetaldehyde

2.

Ethanol

3.

Acetonitrile

4.

Acetone

5.

2-Propanol

6.

2-Methylpentane

7.

3-Methyl pentane

8.

Hexane

9.

Ethyl acetate

10. 2,2-Dimethylpentane
11. 2,4-Dimethylpentane
12. Methylcyclopentane

34

10ppb Nitrosamines in Water: SPME-

GC/MS

96-0142

Chromatogram courtesy of J. Clark, Liggett Group, Inc.

1. Nitrosodimethylamine 

2. Nitrosodiethylamine 

3. Nitrosomethylethylamine 

4. Nitrosodipropylamine 

5. Nitrosopiperidine 

6. Nitrosodibutylamine

7. Nitrosodiphenylamine 

1

2

3

4

5

6

7

Min

4

6

8

1

0

1

2

1

4

1

6

1

8

2

0

2

2

Sample: analytes in (water + 25% KCl, pH 10)

SPME Fiber: 65µm PDMS-DVB

Extraction: immersion, 15 min (rapid stirring)

Desorption: 270°C, 1 min

Column: PTA-5 (amine deactivated,

30m x 0.32mm ID, 0.5µm film)

Oven: 50°C (1 min) to 250°C at 10°C/min, 

hold 2 min

Carrier: helium, 30cm/sec

Det.: GC/MS (quadrupole, SIM)

Inj.: splitless, 250°C (0.75mm ID liner)

35

New Development: Biocompatible Fiber 

Pipette Tips for Solvent Extraction

36

Single Use Biocompatible Fiber Probes 

for in vivo Analysis

37

Comparison of SPME in-vivo PK Study of 

Carbamazepine from Mice Whole Blood to 

Extracts of Plasma Removed from Mice 

Slide Courtesy of Ines de Lannoy-NoAb BioDiscoveries

SPME 1 mouse

Terminal blood draw

Plasma from 3 mice

0

60

120

180

240

300

1

10

100

1000

10000

Time (min)

CB

Z C

oncentration (ng/m

L)

38

Courtesy of 

Joseph Kennedy 

of Prosolia

SPME fiber Holder with Automated 

DESI-1D Source

39

Solid Phase Microextraction (SPME) 

Products

•

Fibers

•

Holders

•

Manual

•

For autosamplers

•

Accessories

•

Instructions

•

Applications on CD

sigma-aldrich.com/spme

40

Sample Prep Innovations

•

Solid Phase Microextraction (SPME)

•

High specificity SPE (SupelMIPs)

•

Dispersive SPE

•

Silver Ion SPE for FAMEs

•

Carbonaceous adsorbents

•

Flash chromatography

Users are...

•

Analytical chemists (LC, LC-MS, GC...)

Interested in...

•

Very selective extraction 

•

Analysis at extremely low concentrations 

(ppb, ppt)

•

Increasing specificity of sample prep from 

complex matrixes

Users can expect...

•

More rigorous washing to remove matrix

•

Detect at lower levels

Users are...

•

Analytical chemists (LC, LC-MS, GC...)

Interested in...

•

Very selective extraction 

•

Analysis at extremely low concentrations 

(ppb, ppt)

•

Increasing specificity of sample prep from 

complex matrixes

Users can expect...

•

More rigorous washing to remove matrix

•

Detect at lower levels

41

High Specificity Sample Prep

•

The specific innovation we will describe:

•

SupelMIP Molecularly Imprinted Polymers

•- SPE tubes
•- 96-well plates

42

The Molecular Imprinting Process

•

Molecularly imprinted polymers (MIPs) are polymers that have been 

prepared by polymerizing either pre-formed or self-assembled monomer-

template complexes together with a cross-linking monomer. After removal 

of the template molecule, a polymer with binding sites for the template is 

obtained. 

43

The MIP Binding Site

•Graphical 

representation of 

the MIP binding 

site, which 

contains a cavity 

of the right size 

and attractive 

molecular 

features that can 

bind to the target 

molecule(s).

44

SupelMIP Chloramphenicol: Analysis in 

Honey

• Chloramphenicol is an antibiotic that is monitored in honey.

Background from honey sample cleaned 

by SupelMIP SPE and LLE for 

Chloramphenicol analysis

0.E+00

1.E+08

2.E+08

3.E+08

0

1

2

3

4

5

Time (min) 

T

IC

 150-

500 M/

Z

MIP
LLE

Position of 

chloramphenicol peak

-1

0

1

2

3

4

5

6

-1

0

1

2

3

4

5

6

theoretical concentration (ng/mL)

ex

p

er

im

e

n

tal

 co

n

ce

n

tr

at

io

n

 (

n

g

/m

L

)

standard

MIP

LLE

generic 
polymer

Comparison of ion suppression effect 

between different clean-up methods for 

honey. Samples were post-spiked with CAP 

prior to analysis.

45

Overview of a Typical SupelMIP SPE 

Procedure

•Very simple methods.
•Full protocols are 

included with each MIP 

product.

•Protocols may require 

optimization depending 

on the sample matrix.

47

SupelMIP Products



PAHs in edible oils



Nitroimidazoles in milk, eggs and other foods



Nonsteroidal anti-inflammatory drugs (

NSAIDS) in 

wastewater and other matrices



Fluoroquinolones in bovine kidney, honey and 

milk



Amphetamines and related compounds in urine



Chloramphenicol in plasma, urine, milk, honey 

and shrimp



NNAL - nitroso compound in urine



TSNAs - tobacco specific nitrosamines in urine 

and tobacco



β

-agonists and β-blockers in tissue, urine and 

wastewater



Clenbuterol in urine



Triazines in water



Riboflavin in milk

sigma-aldrich.com/supelmip

48

Topics: Sample Prep Innovations

•

SPME (solid phase microextraction)

•

High specificity SPE (SupelMIP)

•

Dispersive SPE

•

Silver Ion SPE for FAMEs

•

Carbonaceous adsorbents

•

Flash chromatography

Users are...

•

Food safety analysts

Interested in...

•

Multi-residue pesticide analysis in food 

and agricultural products

Users can expect...

•

Quick, easy, inexpensive extraction 

method

Users are...

•

Food safety analysts

Interested in...

•

Multi-residue pesticide analysis in food 

and agricultural products

Users can expect...

•

Quick, easy, inexpensive extraction 

method

49

Dispersive SPE (dSPE or QuEChERS) 

Multiresidue Pesticide Method

•Multi-residue (100’s) pesticide analysis

•Retains/removes key interferences in food 

samples

•Analytes are un-retained

•

Quick (~30 min./6 samples)

•

Easy (no laborious steps)

•

Cheap

•

Effective (wide scope, low consumption)

•

Rugged (minimal sources of errors)

•

Safe (solvents and techniques)

50

Dispersive SPE Procedure

Procedure:
1. Food initially extracted with aq. miscible 

solvent (e.g. ACN)

2. High amounts of salts (NaCl, Mg-sulfate) 

and buffering agents added to induce 

phase separation and stabilize 

acid/base labile pesticides

3. Shake/centrifuge. Isolate aliquot of sup 

for SPE clean-up.  

4. Transfer supernatant to centrifuge tube.  

Add bulk SPE phase(s) and salts. 

Shake/vortex. Centrifuge and analyze 

supernatant. 

Standard dSPE product line configured for:
• CEN Standard Method EN – 15662

• AOAC Method 2007.01 

Full details of the simple protocol is included with the product.

51

GC-MS of Pesticides from Oranges 

Following Extraction with dSPE

G003590

52

Dispersive SPE Products
• Centrifuge tubes containing pre-

determined amounts of salts and 

SPE sorbents to support the most 

common method configurations 

used today

sigma-aldrich.com/spe

Also available:

• Sample packs

• Custom tubes and packing materials

53

Topics: Sample Prep Innovations

•

SPME (solid phase microextraction)

•

High specificity SPE (SupelMIP)

•

Dispersive SPE

•

Silver Ion SPE for FAMEs (Discovery Ag-Ion)

•

Carbonaceous adsorbents

•

Flash chromatography

Users are...

•

Food analysts

Interested in...

•

Measuring cis/trans fats or degree of 

unsaturation

Users can expect...

•

To fractionate FAME samples prior to GC 

analysis, simplifying analytical 

chromatography and improving method 

accuracy

Users are...

•

Food analysts

Interested in...

•

Measuring cis/trans fats or degree of 

unsaturation

Users can expect...

•

To fractionate FAME samples prior to GC 

analysis, simplifying analytical 

chromatography and improving method 

accuracy

54

Discovery Ag-Ion SPE for FAME 

Fractionation

• Silver ion anchored onto SCX SPE support
• Ag+ forms a charge transfer complex with unsaturated FAME double

bond

•

Ag+ = electron acceptor; double bond = electron donor

• Cis configuration offers greater steric accessibility = stronger retention
• Strength of interaction increases with no. of double bonds

55

Overview Discovery Ag-Ion SPE 

Procedure

1. 1) Fatty acids (FA) extracted from food sample
2. 2) FA converted to FAMEs using BF3 

3. 3) FAMEs are extracted into hexane
4. 4) Hexane sample applied to Discovery Ag-Ion 

SPE cartridge

5. 5) FAMEs separated using different mixtures of 

hexane:acetone to extract from cartridge

•

Increasing % acetone disrupts retention of 

strongly retained FAMEs (cis and higher 

number of double bonds)

6. 6) Fractions analyzed by GC

56

Cis/Trans Fractionation of FAMEs from 

Potato Chips with and without Ag-Ion 

SPE

57

Discovery Ag-Ion SPE Products

http://tinyurl.com/agionspe

58

Topics: Sample Prep Innovations

•

SPME (solid phase microextraction)

•

High specificity SPE (SupelMIP)

•

Dispersive SPE

•

Silver Ion SPE for FAMEs

•

Carbonaceous adsorbents (ENVI-Carbs)

•

Flash chromatography

Users are...

•

Analytical chemists, HPLC, GC doing 

sample prep

Interested in...

•

Extraction of highly polar compounds 

from water samples, and many others...

Users can expect...

•

High extraction efficiency 

Users are...

•

Analytical chemists, HPLC, GC doing 

sample prep

Interested in...

•

Extraction of highly polar compounds 

from water samples, and many others...

Users can expect...

•

High extraction efficiency 

59

Structural Classification of Carbons

60

Carbon Sorbents for Sample Prep
• Packed SPE tubes:

•

Supelclean™ ENVI-Carb PLUS – spherical carbon molecular sieve for 

extraction of highly polar compounds from water samples

•

Supelclean ENVI-Carb-II/PSA SPE – multilayer SPE tubes for multiresidue 

pesticide analysis in foods

•

Supelclean ENVI-Carb-II SPE – isolation/removal of pigments (e.g., chlorophyll 

and carotenoids) and sterols commonly present in fruits, vegetables, and other 

natural products

•

Supelclean ENVI-Carb-II/SAX/PSA SPE – additional ion exchange capability

•

Supelclean PSA SPE – polymerically bonded, ethylenediamine-N-propyl phase 

that contains both primary and secondary amines

Dual Layer Supelclean ENVI-Carb-II/PSA SPE Tube

•

http://tinyurl.com/carbonspe

61

Supelclean ENVI-Carb PLUS

Examples of polar compounds:

Acephate

log P -0.85

Acrylamide

log P -0.67

1,4-Dioxane

log P -0.27

Oxamyl

log P -1.2

Spherical Carbon Molecular Sieve
• Extraction of highly polar 

compounds from water samples

• > 70% Abs Recovery from 0.5 L 

drinking water (1-100 ng/mL)

Procedure:
1. Condition w/ 10 mL MeOH & 10 

mL DI water

2. Load up to 1 L sample
3. Reverse tube & elute w/ 4-5 mL 

MeOH in opposite direction

62

GC-MS Analysis of 1,4-dioxane in water extracted using 

ENVI-Carb Plus

6

8

10

12

14

16

18

20

22

24

Time (min)

1

2

3

• THF-d8 (Int. Std.)

• 1,4-dioxane-d8 (surrogate)

• 1,4-dioxane

Column:  SPB-624, 30 m x 0.25 mm I.D. ,1.4 µm

Oven:  30 °C (1 min.), 7 °C/min. to 90 °C, 20 °C/min. to 200 °C (3 min.)

Inj:  200 °C

Carrier:  helium, 1 mL/min constant flow

Injection:  2 µL, splitless

MS interface:  220 °C

Scan range:  SIM

63

Topics: Sample Prep Innovations

•

SPME (solid phase microextraction)

•

High specificity SPE (SupelMIP)

•

Dispersive SPE

•

Silver Ion SPE for FAMEs

•

Carbonaceous adsorbents (ENVI-Carbs)

•

Flash Chromatography Users are...

•

Synthetic, organic chemists

•

Medicinal chemists

Interested in...

•

Purification of relatively large samples 

from reaction mixtures or other samples

Users can expect...

•

Fast, simple, inexpensive purifications

•

High N (spherical particles)

Users are...

•

Synthetic, organic chemists

•

Medicinal chemists

Interested in...

•

Purification of relatively large samples 

from reaction mixtures or other samples

Users can expect...

•

Fast, simple, inexpensive purifications

•

High N (spherical particles)

64

• Higher efficiency of spherical 

particles translates to 

narrower bands for more 

concentrated fractions and 

faster isolations.

• samples: 5-hydroxy-DL-tryptophan

and DL-tryptophan

• cartridges: 53 mm x 23 mm I.D.

• mobile phase: methanol:water (90:10) 

detection: UV 254 nm

• flow rate: 20 mL/min.

Spherical particles

Irregular particles

80 mL

25 mL

Fraction 1 Volume

260 mL

400 mL

Irregular silica

40 mL

120 mL

Spherical silica

Fraction 2 Volume

Total Volume

Particle Type

Performance of Spherical vs. 

Irregular Silicas in Flash 

Application

65

VersaFlash Support Literature

& Products

• Silica & C18 Cartridges

•

Particle size options

•

Cartridge size options

•

Cartridges can be coupled

•

Reversible

•

Compatible with other systems

• All system components

66

Summary

•Solid Phase Microextraction (SPME) http://www.sigma-aldrich.com/spme
•High specificity SPE (SupelMIPs) http://www.sigma-aldrich.com/supelmip
•Dispersive SPE for pesticide extraction http://www.sigma-aldrich.com/spe
•Silver Ion SPE for FAMEs (Discovery Ag-Ion SPE) 

http://tinyurl.com/agionspe

•Carbon adsorbents for polar compounds (ENVI-Carbs) 

http://tinyurl.com/carbonspe

•Flash chromatography http://www.sigma-aldrich.com/versaflash

67

Acknowledgements/Collaborators

Prof. Janusz Pawliszyn, U. Waterloo, Canada

Ines de Lannoy, NoAb Biodiscovery (in vivo applications)

Joseph Kennedy, Prosolia (DESI)
Supelco and Fluka R&D Teams

For more information on the subjects presented 

here, please contact [email protected] or 

your regional sales team.