[ CARE AND USE MANUAL ]
DisQuE QuEChERS SAMPLE PREPARATION PRODUCTS AND KITS
CONT ENT S
I. INTRODUCTION
I. INT RODUC T ION
Dispersive SPE (d-SPE), commonly referred to as “QuEChERS”, is a simple and straightforward sample preparation technique suitable for multi-residue pesticide analysis in a wide variety of food and agricultural products. The high quality DisQuE™ QuEChERS sample preparation and extraction products contain conveniently-packaged foil pouches and centrifuge tubes in 50 mL, 15 mL, and 2 mL formats which provide the most common buffers and sorbents for QuEChERS methods. For added convenience, kits are available that include methods and consumables for rapid method development and routine analysis.
II.
AVAIL ABL E K IT S
III.
INDIV IDUA L P OUC H E S, E X T RAC T ION T UBE S, C L EANU P T UBE S, AND BU L K S P E SO RBENT S
IV. P ROC E DU R E OV E RV IE W V.
USING T H E AOAC K IT AND M E T HOD
V I. USING T H E C EN K IT AND M E T HOD V II. STO RAG E AND DIS P OSA L OF US E D C A RT RIDG E S V III. A DDIT IONA L INFO RMAT ION IX . O RD E RING INFO RMAT ION X .
LIT E RAT U R E R EF E R ENC E S
[ CARE AND USE MANUAL ]
II. K IT CONT ENT S
Clean-Up Tubes
DisQuE QuEChERS Sample Preparation kits are designed for preparing
Name
Contents
samples for routine multi-pesticide residue analysis. T he kits are
2 mL Tube–White Cap
150 mg MgSO 4, 50 mg PSA
available in the following configurations:
2 mL Tube–Blue Cap
150 mg MgSO 4, 50 mg PSA, 25 mg C18
Kit for AOAC Official Methods
2 mL Tube–Yellow Cap
150 mg MgSO 4, 25 mg PSA
2 mL Tube–Green Cap
150 mg MgSO 4, 25 mg PSA, 25 mg C18
2 mL Tube-Blue Cap
150 mg MgSO 4, 25 mg PSA, 25 mg C18, 7 mg GCB
2 mL Tube-Yellow Cap
150 mg MgSO 4, 50 mg C18
2 mL Tube-Blue Cap
150 mg MgSO 4, 25 mg PSA, 2.5 mg GCB
2 mL Tube-Blue Cap
150 mg MgSO 4, 50 mg PSA, 30 mg C18, 30 mg Al-N
15 mL Tube–White Cap
900 mg MgSO 4, 150 mg PSA
15 mL Tube–Blue Cap
900 mg MgSO4, 150 mg PSA, 150 mg C18
15 mL Tube-Clear Cap
1200 mg MgSO4, 400 mg PSA
15 mL Tube-Blue Cap
1200 mg MgSO4, 400 mg PSA, 400 mg C18
15 mL Tube-Blue Cap
1200 mg MgSO4, 400 mg PSA, 400 mg C18, 400 mg GCB
Name
Description
DisQuE Dispersive SPE Kit–Pouch Format (AOAC Method 2007.01)
Pouch: 1.5 g sodium acetate and 6 g MgSO 4 50 mL Tube: Empty 2 mL Tube: 150 mg MgSO 4 and 50 mg PSA
DisQuE Dispersive SPE Kit–Pouch Format (CEN Method 15662)
DisQuE Dispersive SPE Kit (AOAC Method 2007.01)
DisQuE Dispersive SPE Kit (CEN Method 15662)
Pouch: 1 g trisodium citrate dihydrate, 0.5 g disodium hydrogencitrate sesquihydrate, 1 NaCl and 4 g MgSO 4 50 mL Tube: Empty 2 mL Tube: 150 mg MgSO4, 25 mg PSA, and 25 mg C18 50 mL Tube: 1.5 g sodium acetate, 6 g MgSO 4 2 mL Tube: 150 mg MgSO 4, 50 mg PSA 50 mL Tube: 4 g MgSO 4, 1 g NaCl, 1 g trisodium citrate dehydrate, 0.5 g disodium hydrogencitrate sesquihydrate 2 mL Tube: 150 mg MgSO4, 25 mg PSA, 25 mg C18
15 mL Tube-Clear Cap
900 mg MgSO4, 300 mg PSA
15 mL Tube-Blue Cap
900 mg MgSO4, 300 mg PSA, 300 mg C18
15 mL Tube-Blue Cap
900 mg MgSO4, 450 mg PSA, 300 mg C18, 50 mg GCB
15 mL Tube-Blue Cap
750 mg MgSO4, 250 mg PSA, 150 mg C18, 150 mg Al-N
III. INDIV IDUA L P OUC H E S, E X T RAC T ION T UBE S, C L EANU P T UBE S, AND BU L K S P E SO RBENT S Bulk Sorbent
Extraction Tubes Name
Description
50 mL Empty Tube for QuEChERS Extraction
–
50 mL Tube–Blue Cap (AOAC Method)
1.5 g sodium acetate, 6 g MgSO 4
50 mL Tube–White Cap (CEN Method)
4 g MgSO 4, 1 g NaCl, 1 g trisodium citrate dehydrate, 0.5 g disodium hydrogencitrate sesquihydrate
Name
Qty
Graphitized Carbon Black
25 g
Trifunctionally-bonded C18 Silica
100 g
Sorbent Pouches Name
Contents
DisQuE Pouch (AOAC Method)
1.5 g sodium acetate, 6 g MgSO 4
DisQuE Pouch (CEN Method)
4 g MgSO 4, 1 g NaCl, 1 g trisodium citrate dehydrate, 0.5 g disodium hydrogencitrate sesquihydrate
DisQuE QuEChERS Sample Preparation
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[ CARE AND USE MANUAL ]
IV. P ROC E DU R E OV E RV IE W 1. Sample Comminution T he sample is coarsely cut before pulverization by a food chopper, blender, or other similar device. T he sample size (10–15 g) used
V. USING T H E AOAC K IT AND M E T HOD The following section describes the general steps involved in using a pouch-format DisQuE QuEChERS sample preparation kits for the AOAC (Association of Analytical Communities) procedure.
in the DisQuE procedure is reduced compared with the traditional
Extraction solution preparation
extraction procedures; therefore, it is important to ensure that the
A solution of 1% acetic acid in acetonitrile is prepared by adding 10 mL of glacial acetic acid to 500 mL of acetonitrile in a 1 L volumetric flask. Bring to final volume with acetonitrile. Mix thoroughly.
original sample is thoroughly homogenized. Blending the sample until it reac hes a consistent texture reduces the variation in the sub-sample that will be used for testing and ensures better extraction efficiency. During the homogenization process, the use of cryogenic blending devices, liquid nitrogen, or dry ice is recommended to
1. Sample Comminution
reduce the loss of highly-volatile or thermally-labile pesticides.
The sample is chopped into 2–5 cm 3 portions with a knife, and then pulverized by a food blender. Blend until homogeneous.
2. Sample Extraction/Partitioning T he sub sample is transferred to an empty 50 mL DisQuE extraction
2. Extraction/Partitioning
tube. Depending on whether you are utilizing the AOAC or CEN
Transfer 15 g of the homogenized sub sample into a 50 mL tube and add 15 mL of 1% acetic acid in acetonitrile. Shake the tube vigorously for 1 minute. Pour the contents of the AOAC method salt pouch to the 50 mL tube. Shake the tube vigorously for 30 seconds. Centrifuge the tube at >1500 rcf for at least 1 minute. Caution: exceeding 10,000 rcf may damage, deform, or break the extraction tube.
QuEChERS method, the method appropriate foil pouch containing pre-weighed salts is selected. T he salts are added to the extraction tube followed by the extraction solvent. During mixing, shake, and invert the extraction tube vigorously to ensure that the sample is thoroughly mixed with the extraction buffers contained in the tube. T he shaken sample is centrifuged, and the extract from Tube 1 is used for further clean-up. T he centrifuge rpm and time should be optimized to ensure a solid sample plug and clean extract free from particulate matter. Note: When the samples are mixed with anhydrous anhydrous magnesium sulfate excessive heat may be generated. It is recommended to vent the tube after a few shakes to release any gas pressure.
Tip: For some commodities that contain a high water content, it is recommended that the extraction solvent is added to the 50 mL extraction tubes prior to the addition of the sample. This prevents undesirable caking of the anhydrous magnesium sulfate to the sample.
3. Dispersive Solid-Phase Extraction Transfer 1 mL of top layer extract from Tube 1 into the 2 mL DisQuE Clean-Up Tube 2. Shake vigorously for at least 30 seconds ensuring the sample and sorbents are thoroughly mixed. Centrifuge Tube 2 at >1500 rcf for 1 minute. Caution: exceeding 17,000 rcf may damage, deform, or break the centrifuge tube. Transfer the top extract into and autosampler vial for analysis.
3. Dispersive Solid-Phase Extraction Typically 1 mL aliquot of the top layer extract from the 50 mL extraction tube is transferred to the 2 mL DisQuE clean-up tube. Shake the tube vigorously for at least 30 seconds ensuring the sample and sorbents are thoroughly mixed. Centrifuge the tube at >3000 rcf for 5 minutes. The sample can be analyzed directly or diluted appropriately with a suitable buffer or solvent. Caution: exceeding 17,000 rcf may damage, deform, or break the centrifuge tube.
DisQuE QuEChERS Sample Preparation
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[ CARE AND USE MANUAL ]
V I. ST E P S OF SAM P L E COMINUT ION AND SOLID - P HAS E E X T RAC T ION USING C EN K IT AND M E T HOD The following section describes the general steps involved in using a pouch-format DisQuE QuEChERS sample preparation kits for the CEN procedure.
1. Sample Comminution The sample is chopped into 2–5 cm 3 portions with a knife, and then pulverized by a food blender. Blend until homogeneous.
V II. S TO RAG E AND DIS P OSA L OF US E D C A RT RIDG E S The devices remain stable when stored in their original sealed packaging. To store unused devices in opened pouches, squeeze the air out of the pouch, fold over the open end of the pouch twice, seal with tape, and store in a desiccator. Dispose of used devices safely in accordance with applicable government or local regulations.
V III. A DDIT IONA L INFO RMAT ION
2. Extraction/Partitioning Transfer 10 g of the homogenized sub sample into a 50 mL tube and add 10 mL of acetonitrile. Shake the tube vigorously for 1 minute. Pour the contents of the CEN method salt pouch to the 50 mL tube. Shake the tube vigorously for 30 seconds. Centrifuge the tube at >1500 rcf for at least 1 minute. Caution: exceeding 10,000 rcf may damage, deform, or break the extraction tube.
For more detailed information, consult the Waters Quality Parts,® Chromatography Columns and Supplies Catalog by visiting www.waters.com/catalog, or contact your Waters representative. If you require technical assistance, or have any questions regarding sample preparation, visit www.waters.com or call us at 1-800-252-4752.
3. Dispersive Solid-Phase Extraction Transfer 1 mL of top layer extract from Tube 1 into the 2 mL DisQuE Clean-Up Tube 2. Shake vigorously for at least 30 seconds ensuring the sample and sorbents are thoroughly mixed. Centrifuge the tube at >3000 rcf for 5 minutes. The sample can be analyzed directly or diluted appropriately with a suitable buffer or solvent. Caution: exceeding 17,000 rcf may damage, deform, or break the centrifuge tube.
IX . O RD E RING INFO RMAT ION Description
Cap color
Quantity
Part number
KITS
Description
DisQuE Dispersive SPE Kit–Pouch Format (AOAC Method 2007.01)
Pouch: 1.5 g sodium acetate and 6 g MgSO 4 50 mL Tube: Empty 2 mL Tube: 150 mg MgSO 4 and 50 mg PSA
blue white
100
176002922
DisQuE Dispersive SPE Kit–Pouch Format (CEN Method 15662)
Pouch: 1 g trisodium citrate dihydrate, 0.5 g disodium hydrogencitrate sesquihydrate, 1 NaCl and 4 g MgSO 4 50 mL Tube: Empty 2 mL Tube: 150 mg MgSO 4, 25 mg PSA, and 25 mg C18
blue white
100
176002923
DisQuE Dispersive SPE Kit (AOAC Method 2007.01)
50 mL Tube: 1.5 g sodium acetate, 6 g MgSO 4 2 mL Tube: 150 mg MgSO 4, 50 mg PSA
blue white
100
176001676
DisQuE Dispersive SPE Kit (CEN Method 15662)
50 mL Tube: 4 g MgSO 4, 1 g NaCl, 1 g trisodium citrate dehydrate, 0.5 g disodium hydrogencitrate sesquihydrate 2 mL Tube: 150 mg MgSO 4, 25 mg PSA, 25 mg C18
white green
100
176001903
Continued ⇒
DisQuE QuEChERS Sample Preparation
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O RD E RING INFO RMAT ION (CONT INU E D) Description
Cap color
Quantity
Part number
EXTRACTION TUBES
Description
50 mL Empty Tube for QuEChERS Extraction
–
blue
50
186006814
50 mL tube containing 1.5 g Sodium Acetate and 6 g MgSO4
1.5 g sodium acetate, 6 g MgSO 4
blue
100
186004571
50 mL tube containing 1 g trisodium citrate dihydrate, 0.5 g disodium hydrogencitrate sesquihydrate, 1 g NaCl, and 4 g MgSO4
4 g MgSO 4, 1 g NaCl, 1 g trisodium citrate dehydrate, 0.5 g disodium hydrogencitrate sesquihydrate
white
100
186004837
SORBENT POUCHES
Contents
DisQuE Pouch (AOAC Method)
1.5 g sodium acetate, 6 g MgSO 4
n/a
50
186006812
DisQuE Pouch (CEN Method)
4 g MgSO 4, 1 g NaCl, 1 g trisodium citrate dehydrate, 0.5 g disodium hydrogencitrate sesquihydrate
n/a
50
186006813
CLEAN-UP TUBES
Contents
2 mL tube containing 150 mg MgSO4 and 50 mg PSA
150 mg MgSO 4, 50 mg PSA
white
100
186004572
2 mL tube containing 150 mg MgSO4, 50 mg PSA, and 50 mg C18
150 mg MgSO 4, 50 mg PSA, 25 mg C18
blue
100
186004830
2 mL tube containing 150 mg MgSO4 and 25 mg PSA
150 mg MgSO 4, 25 mg PSA
yellow
100
186004831
2 mL tube containing 150 mg MgSO4, 25 mg PSA, and 25 mg C18
150 mg MgSO 4, 25 mg PSA, 25 mg C18
green
100
186004832
2 mL tube containing 150 mg MgSO4, 25 mg PSA, 25 mg C18, and 7 mg GCB
150 mg MgSO4, 25 mg PSA, 25 mg C18, 7 mg GCB
blue
100
186008071
2 mL tube containing 150 mg MgSO4 and 50 mg C18
150 mg MgSO4, 50 mg C18
yellow
100
186008075
2 mL tube containing 150 mg MgSO4, 25 mg PSA, and 2.5 mg GCB
150 mg MgSO4, 25 mg PSA, 2.5 mg GCB
blue
100
186008076
2 mL tube containing 150 mg MgSO4, 50 mg PSA, 30 mg C18, and 30 mg Al-N
150 mg MgSO4, 50 mg PSA, 30 mg C18, 30 mg Al-N
blue
100
186008081
15 mL tube containing 900 mg MgSO4 and 150 mg PSA
900 mg MgSO 4, 150 mg PSA
white
50
186004833
15 mL tube containing 900 mg MgSO4, 150 mg PSA, and 150 mg C18
900 mg MgSO4, 150 mg PSA, 150 mg C18
blue
50
186004834
15 mL tube containing 1200 mg MgSO4 and 400 mg PSA
1200 mg MgSO4, 400 mg PSA
clear
50
186008072
15 mL tube containing 1200 mg MgSO4, 400 mg PSA, and 400 mg C18
1200 mg MgSO4, 400 mg PSA, 400 mg C18
blue
50
186008073
15 mL tube containing 1200 mg MgSO4, 400 mg PSA, 400 mg C18, and 400 mg GCB
1200 mg MgSO4, 400 mg PSA, 400 mg C18, 400 mg GCB
blue
50
186008074
15 mL tube containing 900 mg MgSO4 and 300 mg PSA
900 mg MgSO4, 300 mg PSA
clear
50
186008077
15 mL tube containing 900 mg MgSO4, 300 mg PSA and 300 mg C18
900 mg MgSO4, 300 mg PSA, 300 mg C18
blue
50
186008078
15 mL tube containing 900 mg MgSO4, 450 mg PSA, 300 mg C18, and 50 mg GCB
900 mg MgSO4, 450 mg PSA, 300 mg C18, 50 mg GCB
blue
50
186008079
15 mL Tube containing 750 mg MgSO4, 250 mg PSA, 150 mg C18, and 150 mg Al-N
750 mg MgSO4, 250 mg PSA, 150 mg C18, 150 mg Al-N
blue
50
186008080
n/a
25 g bulk
186004835
n/a
100 g bulk
WAT035672
BULK SORBENTS Graphitized carbon black Trifunctionally-bonded C18 silica
PSA = Primary Secondary Amine Bonded Silica Al-N = Alumina N
DisQuE QuEChERS Sample Preparation
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[ CARE AND USE MANUAL ]
X . LIT E RAT U R E R EF E R ENC E S Description Beginner’s Guide to SPE (Solid-Phase Extraction)
Literature Code 715003405 www.waters.com/SPEprimer
Sorbent Selection Guide Wall Chart
720002007EN
Food Testing Application Notebook
720002565EN
“A Rapid Method for the Screening and Confirmation of Over 400 Pesticide Residues in Food” Application Note
720002628EN
Lehotay, S.(2007) JAOAC Int., 90(2) 485-520.
©2015 Waters Corporation. Waters, T he Science of W hat’s Possible, and Waters Quality Parts are registered trademarks of Waters Corporation. . DisQuE is a trademark of Waters Corporation. All other trademarks are the property of their respective owners. ©2015 Waters Corporation. Produced in the U.S.A. July 2015 715001888EN Rev E IH-KK-PDF
Waters Corporation 34 Maple Street Milford, MA 01757 U.S.A. T: 1 508 478 2000 F: 1 508 872 1990 www.waters.com