1. No category

[ Care and Use Manual ]
DisQuE QuEChERS SAMPLE PREPARATION PRODUCTS AND KITS
Contents
i. Introduction
I.introduction
Dispersive SPE (d-SPE), commonly referred to as “QuEChERS”,
is a simple and straightforward sample preparation technique
II. Available Kits
suitable for multi-residue pesticide analysis in a wide variety
of food and agricultural products. The high quality DisQuE ™
IIi. INDIVIDUAL POUCHES, EXTRACTION TUBES, CLEANUP
TUBES, AND BULK SPE SORBENTS
QuEChERS sample preparation and extraction products contain
conveniently-packaged foil pouches and centrifuge tubes in 50
iv. Procedure Overview
mL, 15 mL, and 2 mL formats which provide the most common
V.Using THE AOAC Kit and Method
nience, kits are available that include methods and consumables
buffers and sorbents for QuEChERS methods. For added convefor rapid method development and routine analysis.
VI.USING THE CEN KIT AND METHOD
ViI.STORAGE AND DISPOSAL OF USED CARTRIDGES
ViIi. ADDITIONAL INFORMATION
IX.LITERATURE REFEReNCES
X.ORDERING INFORMATION
DisQuE QuEChERS Sample Preparation Products and Kits
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[ Care and Use Manual ]
II. Kit Contents
Clean-Up Tubes
DisQuE QuEChERS Sample Preparation kits are designed for preparing
samples for routine multi-pesticide residue analysis. The kits are
available in the following configurations:
Kit for AOAC Official Methods
Name
Contents
2 mL Tube–White Cap
150 mg MgSO 4, 50 mg PSA
2 mL Tube–Blue Cap
150 mg MgSO 4, 50 mg PSA, 25 mg C18
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
Name
Description
15 mL Tube–White Cap
900 mg MgSO 4, 150 mg PSA
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
15 mL Tube–Blue Cap
900 mg MgSO4, 150 mg PSA, 150 mg C18
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 MgSO4, 25 mg PSA, and 25 mg C18
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
IV.Procedure Overview
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 MgSO4, 25 mg PSA, 25 mg C18
The sample is coarsely cut before pulverization by a food chopper,
Bulk Sorbent
Name
Qty
Graphitized Carbon Black
25 g
Trifunctionally-bonded C18 Silica
100 g
1. Sample Comminution
blender, or other similar device. The sample size (10–15 g) used in
the DisQuE procedure is reduced compared with the traditional extraction procedures; therefore, it is important to ensure that the original
III. INDIVIDUAL POUCHES, EXTRACTION TUBES,
CLEANUP TUBES, AND BULK SPE SORBENTS
sample is thoroughly homogenized. Blending the sample until it
Extraction Tubes
that will be used for testing and ensures better extraction efficiency.
reaches a consistent texture reduces the variation in the sub-sample
Name
Description
During the homogenization process, the use of cryogenic blending
50 mL Empty Tube for
QuEChERS Extraction
–
of highly-volatile or thermally-labile pesticides.
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
devices, liquid nitrogen, or dry ice is recommended to reduce the loss
2. Sample Extraction/Partitioning
The sub sample is transferred to an empty 50 mL DisQuE extraction
tube. Depending on whether you are utilizing the AOAC or CEN
QuEChERS method, the method appropriate foil pouch containing preweighed salts is selected. The salts are added to the extraction tube
followed by the extraction solvent. During mixing, shake, and invert
Sorbent Pouches
the extraction tube vigorously to ensure that the sample is thoroughly
Name
Contents
mixed with the extraction buffers contained in the tube. The shaken
DisQuE Pouch
(AOAC Method)
1.5 g sodium acetate, 6 g MgSO 4
sample is centrifuged, and the extract from Tube 1 is used for further
DisQuE Pouch
(CEN Method)
4 g MgSO 4, 1 g NaCl, 1 g trisodium citrate
dehydrate, 0.5 g disodium hydrogencitrate
sesquihydrate
clean-up. The 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.
DisQuE QuEChERS Sample Preparation Products and Kits
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[ Care and Use Manual ]
VI.STEPS OF SAMPLE COMINUTION AND SOLID-PHASE
EXTRACTION USING CEN KIT AND METHOD
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
The following section describes the general steps involved for a using
undesirable caking of the anhydrous magnesium sulfate to the sample.
DisQuE QuEChERS sample preparation kits for the CEN procedure.
3. Dispersive Solid-Phase Extraction
1. Sample Comminution
A 1 mL aliquot of the top layer extract from the 50 mL extraction
The sample is chopped into 2–5 cm3 portions with a knife, and then
tube is transferred to the 2 mL DisQuE clean-up tube. Shake the tube
pulverized by a food blender. Blend until homogeneous.
vigorously and invert the tube a few times to ensure the extract is
thoroughly mixing with all the solids in the 2 mL tube. The sample
2. Extraction/Partitioning
can be analyzed directly or diluted appropriately with a suitable
Add 10 mL of acetonitrile and the contents of the CEN method salt
buffer or solvent.
pouch to a 50 mL extraction tube. Manually shake a few times to
ensure that no solids are stuck to the bottom of the tube. Transfer
10 g of the homogenized sub sample into the extraction tube. Shake
V.Using THE AOAC Kit and Method
vigorously for 1 minute. Centrifuge the tube at > 1500 rcf for at
The following section describes the general steps involved for a using
least 1 minute. Caution: exceeding 10,000 rcf may damage, deform,
DisQuE QuEChERS sample preparation kits for the AOAC (Association
or break the extraction tube.
of Analytical Communities) procedure.
3. Dispersive Solid-Phase Extraction
Extraction solution preparation
Transfer 1 mL of top layer extract from Tube 1 into the 2 mL DisQuE
A solution of 1% acetic acid in acetonitrile is prepared by adding
Clean-Up Tube 2. Shake vigorously for at least 30 seconds ensuring
10 mL of glacial acetic acid to 500 mL of acetonitrile in a
the sample and sorbents are thoroughly mixed. Centrifuge Tube 2 at
1 L volumetric flask. Bring to final volume with acetonitrile. Mix
> 3000 rcf for 5 minutes. Transfer the top extract into and autosam-
thoroughly.
pler vial for analysis. Caution: exceeding 17,000 rcf may damage,
1. Sample Comminution
deform, or break the centrifuge tube.
The sample is chopped into 2–5 cm portions with a knife, and then
3
pulverized by a food blender. Blend until homogeneous.
VII.STORAGE AND DISPOSAL OF USED CARTRIDGES
2. Extraction/Partitioning
The devices remain stable when stored in their original sealed pack-
Add 15 mL of 1% acetic acid followed by the contents of the AOAC
aging. To store unused devices in opened pouches, squeeze the air
salt pouch to an empty 50 mL extraction tube. Manually shake a few
out of the pouch, fold over the open end of the pouch twice, seal with
times to ensure that no solids are stuck to the bottom of the tube.
tape, and store in a desiccator.
Transfer 15 g of the homogenized sub sample into the extraction
tube. Shake vigorously for 1 minute. Centrifuge the tube at > 1500
Dispose of used devices safely in accordance with applicable govern-
rcf for at least 1 minute. Caution: exceeding 10,000 rcf may dam-
ment or local regulations.
age, deform, or break the extraction tube.
VIII.ADDITIONAL INFORMATION
3. Dispersive Solid-Phase Extraction
For more detailed information, consult the Waters Quality Parts®,
Transfer 1 mL of top layer extract from Tube 1 into the 2 mL DisQuE
Chromatography Columns and Supplies Catalog by visiting
Clean-Up Tube 2. Shake vigorously for at least 30 seconds ensuring
www.waters.com/catalog, or contact your Waters representative.
the sample and sorbents are thoroughly mixed. Centrifuge Tube 2
at > 1500 rcf for 1 minute. Caution: exceeding 17,000 rcf may
If you require technical assistance, or have any questions
damage, deform, or break the centrifuge tube. Transfer the top
regarding sample preparation, visit www.waters.com or call us at
extract into and autosampler vial for analysis.
1-800-252-4752.
DisQuE QuEChERS Sample Preparation Products and Kits
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[ Care and Use Manual ]
IX. LITERATURE REFERENCES
Description
Literature Code
715003405
www.waters.com/SPEprimer
Beginner’s Guide to SPE (Solid-Phase Extraction)
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.
X. ORDERING INFORMATION
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
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
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
15 mL tube containing 900 mg MgSO4 and 150 mg PSA
white
50
186004833
blue
50
186004834
2 mL tube containing 150 mg MgSO4 and 25 mg PSA
150 mg MgSO 4, 25 mg PSA
900 mg MgSO 4, 150 mg PSA
15 mL tube containing 900 mg MgSO4, 150 mg PSA, and 150 mg C18 900 mg MgSO4, 150 mg PSA, 150 mg C18
BULK SORBENTS
Graphitized carbon black
n/a
25 g bulk
186004835
Trifunctionally-bonded C18 silica
n/a
100 g bulk
WAT035672
PSA = Primary Secondary Amine Bonded Silica
DisQuE QuEChERS Sample Preparation Products and Kits
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[ Care and Use Manual ]
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All other countries:
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1 800 252 4752
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© 2012 Waters Corporation. Waters, The Science of What’s
Possible, Waters Quality Parts, and DisQuE are trademarks of
Waters Corporation.
July 2012 715001888 Rev D KK-PDF
DisQuE QuEChERS Sample Preparation Products and Kits
5
Waters Corporation
34 Maple Street
Milford, MA 01757 U.S.A.
T: 1 508 478 2000
F: 1 508 872 1990
www.waters.com