Professional Documents
Culture Documents
4 5
For ionic
Save Time by processing multiple samples simultaneously or automating method • •
species only Specific Selectivity for your target analytes • •
Decreased Solvent Consumption with the highest loadability •
Decreased Blow-down Time with smaller elution volumes •
Decreased Sample Variation with deconditioning resistant sorbent •
Suggested Reversed Phase Ion-Exchange Normal Phase
Retention pH Stable from 1-14 •
Strata-X, XL, C18, Strata-X-C, X-CW, X-A, Strata NH 2 , CN, Si-1,
Mechanism Phenyl, C8 X-AW, XL-C, XL-CW, FL-PR, EPH, AL-N
Ion-Exchange
XL-A, XL-AW, SAX, Table 2a. Select Your Particle and Pore Size
SCX, WCX, NH2, ABW,
Screen-A, Screen-C Strata-X, X-C, X-A, X-CW, X-AW Strata-XL, XL-C, XL-A, XL-CW, XL-AW
Strata-X-C,
X-CW, X-A, X-AW, Particle & Pore Size 33 μm, 85 Å 100 μm, 300 Å
XL-C, XL-CW,
XL-A, XL-AW, SAX, High Concentration Samples •
SCX, WCX, NH2, ABW, Small Target Analytes (< 10 kDa) •
Screen-A, Screen-C
Large Target Analytes (> 10 kDa) •
Large Volume Samples •
Viscous Samples •
Determine the Sorbent Chemistry
Table 3a. Polymer-Based Sorbents Loading Capacities
SPE Analyte Sorbent
Strata-X Sorbent Strata Sorbent Sample Matrix Sorbent Mass Strata-X, X-C, X-CW, X-A, X-AW Strata-XL, XL-C, XL-CW, XL-A, XL-AW
Mechanism Functional Group Functional Group
R R Blood, serum, plasma 30 mg 250 µL 125 µL
hydrocarbon hydrocarbon C18-E, C18-U, C8 Urine 30 mg 1 mL 500 µL
Reversed Phase X, XL C18-T Filtered tissue homogenates 60 mg 100 mg 50 mg
Phenyl, SDBL
Environmental Samples Sorbent Mass Strata-X, X-C, X-CW, X-A, X-AW Strata-XL, XL-C, XL-CW, XL-A, XL-AW
aromatic aromatic
Water (particulate-free) drinking 200 mg 100 - 400 mL 50 - 200 mL
R - OH CN
hydroxyl polar CN, NH2 Water (particulate-laden) rivers, runoff, etc. 500 mg 100 - 400 mL 50 - 200 mL
Normal Phase
R - NH2 OH Si-1, CN, EPH Soil extracts 500 mg 100 g 50 g
amino polar
Table 4a. Sorbent Wash and Elution Volumes*
NR4+ strong -O2C—weak X-CW, XL-CW WCX The volume of solvent needed for the wash and elution steps is directly related to the mass of sorbent in the SPE tube and more specifically the
RNH3+ weak -O3S—strong X-C Screen-C, SCX “bed volume” of the SPE device. Typically 4 – 16 bed volumes are used in SPE methods.
Ion-Exchange
RSO3- strong +
H3N—weak X-AW, XL-AW NH2
RCO2- weak +
R3N—strong X-A, XL-A Screen-A, SAX
10 mg 30 mg 60 mg 100 mg 150 mg 200 mg 500 mg 1g 2g 5g 10 g
Sorbent Mass
*The elution volumes are specific to the chemical nature of the analyte being extracted, its concentration in the sample, the chemical nature of
Continue to Page 5 Continue to Page 6 the eluting solvent and the bed mass used. The above is a guideline. An elution study should be conducted to determine the appropriate volume
to use.
Strata-X Continue to Page 7
6 7
Sorbent Properties
Filtered tissue homogenates 100 mg sorbent per 100 mg tissue Sample Matrix
Environmental Samples Sorbent Mass
Water (particulate-free) drinking 500 mg/100 mL - 500 mL sample Water
Buffer to appropriate pH and filter particulates from sample.
Water (particulate-laden) rivers, runoff, etc. 1 g/100 mL - 500 mL sample (waste, river, etc.)
Soil extracts 1 g/100 g of soil extract
Homogenize with organic or aqueous solvent depending upon analyte
Table 3b. Sorbent Wash and Elution Volumes* Soil, Sludge
solubility. Settle, decant and filter supernatant; perform Soxhlet extraction.
The volume of solvent needed for the wash and elution steps is directly related to the mass of sorbent in the SPE tube and more specifically the
“bed volume” of the SPE device. Typically 4 – 16 bed volumes are used in SPE methods. Oil-based
Dissolve in non-polar organic (hexane) and extract via polar SPE.
10 mg 50 mg 100 mg 150 mg 200 mg 500 mg 1g 2g 5g 10 g Ointments, Creams Water-based
Sorbent Mass Dissolve in water or water miscible organic (methanol) and extract via
non-polar SPE.
Practical Minimum Wash and
60 µL 300 µL 600 µL 900 µL 1.2 mL 3 mL 6 mL 12 mL 30 mL 60 mL
Elution Volume 4 bed volumes Homogenize with organic or aqueous solvent depending upon analyte
solubility and filter supernatant. Use appropriate SPE mechanism for
Fruit, Vegetable,
Recommended Wash and the dissolution solvent (hexane = polar mechanism; aqueous = non-
120 µL 600 µL 1.2 mL 1.8 mL 2.4 mL 6 mL 12 mL 24 mL 60 mL 120 mL Herbs
Elution Volume 8 bed volumes polar mechanism; methanol/ACN = either non-polar or polar after proper
dilution).
*The elution volumes are specific to the chemical nature of the analyte being extracted, its concentration in the sample, the chemical nature of the eluting solvent and the
bed mass used. The above is a guideline. An elution study should be conducted to determine the appropriate volume to use.
Strata-X Strata
Sample Preparation Support at Your Fingertips
Dedicated sample preparation
team available to assist your
method development needs
8 S 9 S
n
n
O
.. O Condition
) ) ) ) ) )) ))) ) )) ) ) ) ) ) ) )
N
Strata-X ..
Reversed Phase Polar and Non-Polar Oasis® HLB 1 mL Methanol
n
N..
O
N
n O O
)
n
O
) )
n
n
O..S
N
O-
Reversed Phase and Equilibrate
Strata-X-C S O- Bases Oasis MCX
S O O-
Strong Cation-Exchange 1 mL Water
O
O
O ..
n
N
)
n S O O- Reversed Phase and Bases (including
Load
) )
Strata-X-CW n
n
OO
Oasis WCX
O
OH Weak Cation-Exchange Quaternary Amines)
O
OH
Diluted Sample
H
nn
n
O
CH3 Reversed Phase and
Strata-X-A Acids Oasis MAX
) )
n
NH
n
Reversed Phase and Acids (including
)
Strata-X-AW Oasis WAX
Weak Anion-Exchange Sulfonic acids)
S O-
NH NH2
)
nn
n
O
O Elute
)) ) )) )
O
Large Particle Reversed 2x 500 µL 2 % Formic Acid in Methanol/Acetonitrile
Strata-XL ..
.... N Polar and Non-Polar Oasis HLB
)
Phase
O
N
N
O
nn n
n
O
O
O
Large Particle Reversed
)))) ))))
S --O-
Strata-XL-C SS O
.. O Phase and Strong Bases Oasis MCX
NO
OO Cation-Exchange
n n
O
Large Particle Reversed
Bases (including
n
nn O
)) )) )) ))
Strata-XL-CW SOO O-
Phase and Weak Cation- Oasis WCX
O Quaternary Amines) O
)
OOOH H
H Exchange
n
n Large Particle Reversed
nn n
)))) ) )))) )
OCH3
Strata-XL-A Phase and Strong Acids Oasis MAX
NH
N+
O NHNH2
NH3 H NH22 OH
)
NH
CH Anion-Exchange
Large Particle Reversed
n
Acids (including
)
)
NH NH2
)
SPE Method Development Tool Search Hundreds of Applications
Develop SPE methods for sample cleanup and concentration in under one minute. Know the name of your analyte? Immediately find key Sample Prep applications for small molecules and
www.phenomenex.com/mdtool biomolecules by entering the name or the chemical properties of the analyte.
www.phenomenex.com/applications
*Based on 30 mg/1 mL sorbent mass. The above is a convenient starting point for SPE method development. Further optimization may be required to tailor the method to your specific needs.
10 Ste 11 Ste
Strata-X-C / Strata-XL-C
n O Strata-X-A / Strata-XL-A
)
Polymeric SPE
Strong Cation-Exchange & Reversed Phase Strong Anion-Exchange & Reversed Phase
..
N
)
For Bases with pKa ≤ 10.5 Strong Cation-Exchange: For Acids with pKa > 2 Strong Anion-Exchange:
Condition
sulfonic acid ligand Condition di-methylbutyl quaternary
1 mL Methanol 1 mL Methanol amine ligand
O
Equilibrate n Equilibrate
1 mL Water, pH 6-7
)
1 mL Acidified Water
)
S O- CH3
-C
-A
Load Load N+
)
Diluted Acidified Sample Diluted Sample pH 6-7
)
O CH3
Wash 1 Wash 1
1 mL 0.1 N HCI in Water 1 mL 25 mM Ammonium Acetate Buffered, pH 6-7
(collect this fraction to analyze Polar Neutrals)
)
Wash 2
Wash 2 1 mL Methanol CH3
n (collect this fraction to analyze Neutral/Bases)
1 mL 0.1 N HCI in Methanol
O N+
)
)
(collect this fraction to analyze Neutrals/Acids)
Elute Acids CH3
2x 500 µL 5 % Formic Acid in Methanol
Elute Bases OH
)
)
)
NH2
NHCH3
)
+
N
)
Strata-X-CW / Strata-XL-CW Strata-X-AW / Strata-XL-AW CH3
n
)
Weak Cation-Exchange & Reversed Phase Weak Anion-Exchange & Reversed Phase
)
For Bases with pKa > 8 NH2 For Acids with pKa ≤ 5
Weak Cation-Exchange:
NH Weak Anion-Exchange:
NH
NH2
)
)
Condition Condition
1 mL Methanol 1 mL Methanol
Equilibrate Equilibrate
)
)
1 mL Water, pH 6-7 1 mL Water, pH 6-7
O
-AW
-CW
NH2
Load Load NH
)
)
Wash 2
1 mL Methanol
O Wash 2
1 mL Methanol
(collect this fraction to analyze Neutrals/Acids)
)
OH
Elute Any Acid Elute Weak Acids
Elute Any Base Elute Weak Bases 2x 500 µL 5 % NH4OH in Methanol 2x 500 µL 5 % Formic Acid in Methanol
2x 500 µL 5 % Formic Acid in Methanol 2x 500 µL 5 % NH4OH in Methanol
)
*Based on 30 mg/1 mL sorbent mass. The above is a convenient starting point for SPE method development. Further optimization may be required to tailor the method to your specific needs. *Based on 30 mg/1 mL sorbent mass. The above is a convenient starting point for SPE method development. Further optimization may be required to tailor the method to your specific needs.
O
Phenomenex l WEB: www.phenomenex.com Phenomenex l WEB: www.phenomenex.com
)
b b
12
Step 3 General Starting Methods: Strata®
13
Step 3 General Starting Methods: Strata® (cont’d)
® ® ® ® ® ® ®
Recommended Method Waters Agilent SampliQ Biotage UCT CleanScreen Supelco
Strata Phase Phase Benefits Sorbent Chemistry ® ® ® ®
( See pp. 16-17) Sep-Pak Bond Elut IST® ISOLUTE StyreScreen® Discovery
O
O
Si
METHOD SampliQ C18EC
C18-E Extraction of hydrophobic molecules O
O
1 C8 C8(EC) C8 DSC-8
C18-E O
Si
O
Si
Bond Elut C8
O
O
Si
METHOD SampliQ Phenyl
Phenyl (PH) Extraction of aromatic compounds O 1 PH Phenyl DSC-Ph
O
Si Si
Bond Elut PH
O O
O
O
Si C
METHOD SampliQ Cyano (CN)
CN Extraction of polar compounds O
N
1 CN CN CN DSC-CN
Bond Elut Cyano (CN-E)
O
Si OH
O
n SampliQ DVB
Extraction of non-polar and polar compounds;
)
METHOD
SDB-L 1 Bond Elut ENV 101 StyreScreen® DVB DSC-PS/DVB
pH resistant sorbent
Bond Elut LMS
)
METHOD ®
SampliQ Florisil® PR ®
FL-PR (Florisil®) Extraction of pesticides Florisil 6 Florisil FL Florisil® PR ENVI-Florisil
Bond Elut Florisil®
O
O
Si NH2
METHOD SampliQ Amino (NH2)
NH2 Extraction of strong anions O
6 NH2 NH2 Amino Propyl DSC-NH2
Bond Elut Aminopropyl (NH2)
O
Si NH2
O
O
O
Si C
METHOD SampliQ Cyano (CN)
CN Extraction of polar compounds O
N
6 CN CN CN DSC-CN
Bond Elut Cyano (CN-E)
O
Si OH
O
® ® ® ® ® ® ®
Recommended Method Waters Agilent SampliQ Biotage UCT CleanScreen Supelco
Strata Phase Phase Benefits Sorbent Chemistry ® ® ® ® ®
( See pp. 16-17) Sep-Pak Bond Elut IST ISOLUTE StyreScreen® Discovery
O
O O
S
O
Si
Inquire
ABW
O
O
NH2
O
O N
Si
O
METHOD SampliQ Si-SAX
SAX Extraction of weak anions O
Si OH
5 Accell Plus QMA SAX Quaternary Amine DSC-SAX
O
Bond Elut SAX
O
O
SampliQ Si-SCX
O
Si
S O
METHOD
SCX Extraction of 1°, 2°, and 3° amines O
O
O
O
O
Si OH
METHOD
WCX Extraction of quaternary amines O
O
3 Accell Plus CM Bond Elut CBA CBA Carboxylic Acid DSC-WCX
Si OH
O
O
O O SampliQ C8/Si-SCX Mixed
Mixed-mode cation-exchange that also provides
S
O
Screen-C
Si
O
METHOD Mode HCX Clean Screen® DAU
hydrophobic retention O
O
3
Bond Elut Certify®
Si
O
O
O O
O
O N
Mixed-mode anion-exchange that also provides
Si
METHOD
Screen-A O
5 Bond Elut Certify® II HAX Clean Screen THC
hydrophobic retention O
Si
O
O
O
Si NH2 SampliQ Amino (NH2)
NH2 Extraction of strong anions O
NH2 NH2 Amino Propyl DSC-NH2
O
Si NH2 METHOD Bond Elut Aminopropyl (NH2)
O
4
Special Sorbents
EPH O
O
O
METHOD
Petroleum hydrocarbons from environmental samples O
Si OH
6
Hydrocarbons) O
Strata Reversed Phase METHOD Strata NH2 (WAX) Weak Anion - Exchange
METHOD Solid Phase Extraction
Condition
1 Condition
4
1 mL Methanol 1 mL Methanol
Equilibrate Equilibrate
1 mL DI Water 1 mL Water, pH 6-7
Load Load
Pretreated sample Pretreated sample, pH 6-7
Wash Wash 1
1 mL 5 % Methanol in DI Water, dry under vacuum for 2-5 min 1 mL 25 mM Ammonium Acetate Buffer, pH 6-7
Elute Wash 2
1 mL Methanol 1 mL Methanol, dry under vacuum for 2-5 min
2
Condition Strata SAX Strong Anion - Exchange
METHOD
1 mL Methanol
5
Condition
Equilibrate
1 mL Methanol
1 mL DI Water, pH 6-7
Equilibrate
Load
1 mL Water
Pretreated sample, pH 6-7
Load
Wash 1
Pretreated sample, pH 6-7
1 mL Water, pH 6-7
Wash 2 Wash 1
1 mL Methanol, dry under vacuum for 2-5 min 1 mL 25 mM Ammonium Acetate Buffer, pH 6-7
Elute
Strata SCX Strong Cation - Exchange
METHOD
1 mL 5 % Formic Acid in Methanol
Condition
3
1 mL Methanol Strata Strata Normal Phase Method
METHOD
Condition
6
Equilibrate
1 mL Acidified Water IPA / DCM
Load Equilibrate
Pretreated sample (acidified) Hexane
Wash 1 Load
1 mL 0.1N HCl in Water Pretreated sample
Wash 2 Wash
1 mL 0.1N HCl in Methanol, dry under vacuum for 2-5 min 5 % DCM in Hexane
Elute
1 mL 5 % NH4OH in Methanol Elute
1:1 Hexane / DCM or 1:1 Hexane / IPA
Preventing Analyte Loss by Skipping the Dry Down Step using Microelution SPE Improved Clean Up and Recovery of Pharmaceutical Compounds From Plasma:
SPE vs. Liquid-Liquid Extraction
Many target analytes, such as peptides and thermolabile compounds, can be lost during dry down steps. Stop Although liquid-liquid extraction (LLE) has been frequently used in the past, newer techniques with improved
risking analyte loss and skip the dry down, without losing sensitivity using Strata®-X microelution plates. A specificity towards particular analytes have allowed analysts to improve recovery and reproducibility of their
new format that provides increased sensitivity for analytes of interest. samples. It was found that SPE provides cleaner extracts, higher recoveries, and better reproducibility which
can greatly improve results when working with pharmaceutical compounds from plasma.
2x 25 µL Trifluoroacetic acid/acetonitrile/water Dry down Dry down @ 53 °C under a stream of nitrogen for 20 minutes
Elute 2x 175 µL Trifluoroacetic acid/acetonitrile/water (1:74:25)
(1:74:25) Reconstitute Reconstitute in 500 µL of mobile phase
Dry down under a gentle stream of Nitrogen and
Dry Down reconstitute in 50 µL Trifluoroacetic acid/ acetonitrile/water NOT REQUIRED
(1:74:25) Chromatogram after SPE Extraction from a Plasma Matrix
Inject 10 µL 10 µL
140
Column: Kinetex® 2.6 µm C18
2 Dimensions: 75 x 4.6 mm
120 Part No.: 00C-4462-E0
DALDA C8 (peptide) Extracted from Serum Mobile Phase: Water (adjusted to pH 3.3 with
phosphoric acid)/Methanol (63:37)
22996 100 Flow Rate: 1.5 mL/min
Temperature: 30 °C
1.7e5 Detection: UV @ 254 nm
22997 80
Sample: 1. Flurbiprofen (IS)
1.6e5
1.6e5 2. Diclofenac
Microelution SPE
mAU
1.5e5
1.5e5
• Skip the dry down 60 1
1.4e5
1.4e5 and increase recovery
1.3e5 Column: Kinetex 5 μm C8
®
• Absolute Recovery: 95 %
1.3e5
Dimensions: 50 x 4.6 mm 40
1.2e5
1.2e5 Part No.: 00B-4608-E0
• % CV (N=6): 5.7
App ID 19701
1.1e5
1.1e5 Mobile Phase: A: 0.1 % Formic acid in Water
20
B: 0.1 % Formic acid in Methanol
cps
1.0e5
1.0e5
Gradient: Time (min) %B
Intensity,Intensity,
9.0e4
9.0e4 0.00 10 0
cps
8.0e4
8.0e4 3.00 90 10 mg SPE
4.00 90 2.0 3.0 4.0 5.0 min
7.0e4
7.0e4 • ~50 % loss is observed
4.01 10 after dry down step
6.0e4
6.0e4
App ID 22996 and 22997
6.00 10
• Absolute Recovery: 50 %
5.0e4
5.0e4 Flow Rate: 600 μL/min
Temperature: Ambient • % CV (N=6): 10.5
4.0e4
4.0e4
Detection: MS/MS, Triple Quad™ 4500 (SCIEX), ESI+ To learn more about this method and others, visit:
3.0e4
3.0e4 Sample: DALDA C8 (peptide), spiked at 10 ng/mL www.phenomenex.com/SPE
2.0e4
2.0e4
1.0e4
1.0e4
0.0
0 0.5 11
1 1.5 2 2.5 3 3.5 4 4.5 5 5.5 min
min
Amphetamines from Urine Using Microelution SPE Urinary Steriods using Strata®-X SPE
An extraction method to isolate five amphetamines from urine using Strata®-X-C Microelution 96-well We evaluated a variety of silica-based and polymer-based SPE sorbents for the quantification of cortisol,
SPE plates followed by LC/MS/MS analysis. By utilizing the microelution SPE format, the dry down step cortisone, prednisolone, and prednisone, each of which provides a different retention mechanism. The
was skipped saving at least 30 minutes without negatively impacting the sensitivity of our analysis. The five evaluation showed that the Strata-X polymer-based SPE sorbent, with a unique elution solvent has been
amphetamines were accurately quantified at detection levels down to 25 % below the cutoff levels specified found to be a robust, reproducible, and cost effective sample preparation solution for the laboratory in human
by the Substance Abuse and Mental Health Services Administration (SAMHSA). urine for all four corticosteroids.
Recovery (%)
100
60
MDA 62.25 2.15 106 4.2 80
50
Recovery %
40
MDMA 62.25 2.36 99 15.7
60 30
6.00 10
4.5e4 Flow Rate: 500 µL/min
Intensity, cps
80 80
Recovery %
4.0e4 Temperature: Ambient
Detection: MS/MS, Triple Quad™ 4500 (SCIEX), ESI+
Recovery (%)
60
3.5e4 60
3.0e4
40
2.5e4 40
selected
2.0e4
App ID 22986
20
1.5e4 20
0
1.0e4 0% 10% 20% 30% 40% 50% 80% 100%
5000.0 0
% Methanol Cortisone Cortisol Prednisone Prednisolone
0.0
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 min Cortisone Cortisol Prednisone Prednisolone
QCL QCH
Chlorinated Pesticides in Poultry Tissue Using Strata® Alumina-N SPE Phenylbutazone in Ground Meat using Strata®-X-A SPE
Animals used for food consumption are exposed to contaminants at levels that can pose harm to the human population. A simple yet effective SPE and cleanup method for phenylbutazone from meat with recovery values > 90 %.
Presented is a method developed using Strata Alumina-N SPE and GC/ECD for pesticides analysis from poultry fat. This Highly specific LC/MS/MS data is generated using a Kinetex core-shell column enabling rapid run times under
method improves upon the traditional procedure by reducing time and increasing accuracy and reliability. 5 minutes with excellent precision and accuracy.
Pretreatment Protocol
SPE Protocol
1.
Using 1 minute intervals with a microwave, render poultry fat pads ensuring the sample does not
exceed 100 °C
Strata-X-A, 100 mg/6 mL Phenylbutazone and
Weigh 1 gram of rendered fat into a 10 mL volumetric flask and bring to volume with hexane
Part No. 8B-S123-ECH Phenylbutazone-D10
2. Condition 3 mL Methanol
containing internal standards 1 and 2 Chemical Structures
3. Vortex or shake volumetric flasks to ensure proper mixing Equilibrate 3 mL DI Water
Load 4 mL of Pretreated sample CH3
CH3
Wash 1
SPE Protocol 2 mL D.I. Water
Wash 2 2 mL Acetonitrile H
H
Strata Alumina-N, 2 g/12 mL O O
Wash 3 2 mL Ethyl Acetate O O
Part No. 8B-S313-KDG N N D
Dry 5 minutes under full vacuum N N
D
Condition Methanol/Water (86:14) at 10 mL/min until dry D D
Elute 2x 1.5 mL 1 % Formic Acid in Methanol D D
Equilibrate Petroleum ether at full cartridge volume at 10 mL/min D D D
Dry Down Evaporate under a stream of nitrogen gas at 50 °C to dryness D
Load 1 mL Pretreated sample
Reconstitute Resuspend the residue with 500 μL of Methanol/ 0.1 % Formic Acid (50:50)
Elute Ethyl Ether/Petroleum Ether (1.5:98.5) at full cartridge volume and collect eluent
Dry Down Dry down at ambient temperatures under a stream of nitrogen and evaporate to dryness
Reconstitute 2 mL Hexane
Chromatogram
21871
of 10 ppb Phenylbutazone % Recovery of Phenylbutazone
GC / EDC Analysis of Chlorinated Hydrocarbons from Beef Extract at 5 ppb and 75
12 Columns: Zebron™ ZB-MultiResidue™-1 1.24e5 1
Column:
Dimensions:
Kinetex® 2.6 µm XB-C18
50 x 2.1 mm ppb (µg/kg) n=4
Hz Dimensions: 30 m x 0.32 mm x 0.50 µm 1.20e5 Part No.: 00B-4496-AN
Part No.: 7HM-G016-17
Mobile Phase: A: 0.1 % Formic acid in Water Spiked Conc. %CV Accuracy
1800 Injection: Splitless @ 250 °C, 1.0 µL B: 0.1 % Formic acid in Methanol
1.10e5
Carrier Gas: Helium (ramped flow) 5 8.02 100.7
Gradient: Time (min) %B
1 2,3 3.4 mL/min for 6 min ,ramp 5 mL/min to 8 mL/min, hold 12.08 min
Oven Program: 150 °C for 0.5 min to 220 °C @ 20 °C/min to 310 °C @ 6 °C/min 0.00 50
1.00e5
0.50 50 75 5.0 90.3
1600 Detector: ECD @ 350 °C
Makeup Gas: 40 mL/min (N2) 2.00 95
Analytes: 1. 2,4,5,6-Tetrachloro-m-xylene (IS 1) 9.00e4 3.50 95
2. α-BHC 3.51 50
3. Hexachlorobenzene 8.00e4 5.00 50
1400 4. Lindane Flow Rate: 450 µL/min
Intensity, cps
11 5. Heptachlor Column Temp: 45 °C
6. Dursban® (Chlorpyrofos) 7.00e4
Backpressure: 3670 psi (253 bar)
7. Aldrin
1200 8. Heptachlor Epoxide Detection: MS API 4000™ (SCIEX)
9. p,p’-DDE 6.00e4 Samples: 1. Phenylbutazone-d10 (IS)
4 10. Dieldrin 2. Phenylbutazone
9 14 11. o,p-DDT 5.00e4 3. Solvent/MP Impurity
1000 12. p,p’-DDE
13. Endrin
14. p,p’-DDT 4.00e4
15. Methoxychlor
7 16. Mirex
5 3.00e4
800 13 17. Decachlorobiphenyl (IS 2)
8 10
App ID 21871
2.00e4
2
600
App ID 23100
1.00e4
6 17 3
15
0.00
0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8 3.0 3.2 3.4 3.6 3.8 4.0 4.2 4.4 4.6 4.8 min
400
16
2 4 6 8 10 12 14 16 18 min
Polycyclic Aromatic Hydrocarbons using Strata® PAH as Compared to EPA Method 550.1
Polycyclic aromatic hydrocarbon compounds (PAHs) are effectively extracted from water samples while Strata® -X Polymeric SPE Sorbents
humic acids, which often interfere with chromatographic separation, are removed from the sample using Tubes 1 mL (100/box) 3 mL (50/box) 6 mL (30/box)
a SPE sorbent, Strata PAH. It was also found that Strata PAH provides consistent, high recoveries of all 16 Phase 30 mg 60 mg 60 mg 200 mg 500 mg 100 mg 200 mg 500 mg Polymeric SPE
analytes listed under EPA Method 550.1. Strata-X 8B-S100-TAK 8B-S100-UAK 8B-S100-UBJ 8B-S100-FBJ 8B-S100-HBJ 8B-S100-ECH 8B-S100-FCH 8B-S100-HCH
Strata-X-C 8B-S029-TAK — 8B-S029-UBJ 8B-S029-FBJ 8B-S029-HBJ 8B-S029-ECH 8B-S029-FCH 8B-S029-HCH
SPE Protocol Strata-X-CW 8B-S035-TAK — 8B-S035-UBJ 8B-S035-FBJ 8B-S035-HBJ 8B-S035-ECH 8B-S035-FCH 8B-S035-HCH
Strata-X-A 8B-S123-TAK — 8B-S123-UBJ 8B-S123-FBJ 8B-S123-HBJ 8B-S123-ECH 8B-S123-FCH 8B-S123-HCH
Strata PAH, 1.5 g/6 mL
Strata-X-AW 8B-S038-TAK — 8B-S038-UBJ 8B-S038-FBJ 8B-S038-HBJ 8B-S038-ECH 8B-S038-FCH 8B-S038-HCH
Part No. 8B-S130-7CH
Strata-XL 8B-S043-TAK — 8B-S043-UBJ 8B-S043-FBJ 8B-S043-HBJ 8B-S043-ECH 8B-S043-FCH 8B-S043-HCH
Condition 20 mL Dichloromethane, 20 mL Methanol, 20 mL D.I. Water Strata-XL-C 8B-S044-TAK — 8B-S044-UBJ 8B-S044-FBJ 8B-S044-HBJ 8B-S044-ECH 8B-S044-FCH 8B-S044-HCH
Load 100 µL PAH standards (100 µg/mL in Acetonitrile) spiked into 100 mL Water/Acetonitrile (75:25) Strata-XL-CW 8B-S052-TAK — 8B-S052-UBJ 8B-S052-FBJ 8B-S052-HBJ 8B-S052-ECH 8B-S052-FCH 8B-S052-HCH
Wash 5 mL Methanol/D.I. Water (50:50) Strata-XL-A 8B-S053-TAK — 8B-S053-UBJ 8B-S053-FBJ 8B-S053-HBJ 8B-S053-ECH 8B-S053-FCH 8B-S053-HCH
Strata-XL-AW 8B-S051-TAK — 8B-S051-UBJ 8B-S051-FBJ 8B-S051-HBJ 8B-S051-ECH 8B-S051-FCH 8B-S051-HCH
Dry 15 seconds under 10” Hg Vacuum
Elute 6 mL Dichloromethane Strata Silica-Based SPE Sorbents
®
3 .5e 8 Adapter Caps assembly, polypropylene lid with gasket, male and female
Sample: Humic Acids from Suwannee River
Part No. Description Unit luers and yellow end plugs, stopcock valves, collection rack
3 .0e 8
AH0-7191 Adapter Caps for 1, 3, and 6 mL SPE tubes, polyethylene, with Luer tip 15/pk assemblies, polypropylene needles, lid support legs. Waste
2 .5e 8
container included with 12-position manifold.
PAH
trata
App ID 19662
2 .0e 8
S (1) The 10-position Tall Boy Vacuum Manifold Collection Rack
from SPE Tube Vacuum Manifolds includes 4 plates: one base plate, one dimple plate, one small
act
Extr
1 .5e 8 plate and one large plate and three riser bar legs, along with 12
Part No. Description Unit
id
i c ac 24 - Position Vacuum Manifold*3
manifold clips to support the plates. The assembly also includes 10 polypropylene needles, 10
Hum
1 .0e 8
stopcocks and 4 black legs to support the lid when taken off the glass block.
AH0-6024 SPE 24-Position Vacuum Manifold Set, complete assembly ea
5 .0e 7
12 - Position Vacuum Manifold*2 (2) The 12-position Collection Rack Assembly consists of 3 support legs, base plate, dimple plate,
0 .0 AH0-6023 SPE 12-Position Vacuum Manifold Set, complete assembly ea small plate, medium plate, large plate, volumetric plate, and 12 retaining clips.
3.00 3 .0 5 3.10 3.15 3.20 3 .2 5 3.30 3.35 3 .40 3 .4 5 3.50 3.55 3 .6 0 3.65 3.70 3.75 3 .8 0 3.85 3.90 3.95 min
10 - Position Tall-Boy™ Vacuum Manifold*1
(3) The 24-position Collection Rack Assembly consists of 3 support legs, base plate, dimple plate,
AH0-7502 SPE 10-Position Tall-Boy Vacuum Manifold, complete assembly ea small plate, large plate, and 12 retaining clips.
Australia Luxembourg
t: +61 (0)2-9428-6444 t: +31 (0)30-2418700
f: +61 (0)2-9428-6445 f: +31 (0)30-2383749
auinfo@phenomenex.com nlinfo@phenomenex.com
Austria Mexico
t: +43 (0)1-319-1301 t: 01-800-844-5226
f: +43 (0)1-319-1300 f: 001-310-328-7768
anfrage@phenomenex.com tecnicomx@phenomenex.com
Italy
t: +39 051 6327511
f: +39 051 6327555
italiainfo@phenomenex.com
www.phenomenex.com
Phenomenex products are available worldwide.
For the distributor in your country, contact Phenomenex USA,
International Department at international@phenomenex.com
Trademarks
Strata and Kinetex are registered trademarks of Phenomenex. Zebron, Tall-Boy, SecurityGuard,
MultiResidue, and Presston are trademarks of Phenomenex. Agilent, Bond Elut, SampliQ are
registered trademarks of Agilent Technologies. Waters, Oasis, and Sep-Pak are registered
trademarks of Waters Corp. Supelco and Discovery are registered trademarks of Sigma-Aldrich, Co.
LLC. UCT is a registered trademark of United Chemical Technologies. Biotage, IST, and Isolute are
registered trademarks of Biotage. Dursban is a registered trademark of Dow Agro Sciences LLC.
Triple Quad and API 4000 are trademarks of AB SCIEX Pte. Ltd. AB SCIEX™ is being used under
license.
Disclaimer
BR41280317_W
Phenomenex is not affiliated with Waters Corp., Sigma Aldrich, Co. LLC., United Chemical Technol-
ogies, or Biotage.