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SN/T 0337-2019: (Determination of carbofuran and its metabolite residues in foods of plant origin for export Liquid chromatography-mass spectrometry / mass spectrometry)
Status: Valid SN/T 0337: Evolution and historical versions
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
| SN/T 0337-2019 | English | 299 |
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(Determination of carbofuran and its metabolite residues in foods of plant origin for export Liquid chromatography-mass spectrometry / mass spectrometry)
| Valid |
SN/T 0337-2019
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| SN 0337-1995 | English | 279 |
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Method for the determination of carbofuran residues in fruits and vegetables for export
| Obsolete |
SN 0337-1995
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PDF similar to SN/T 0337-2019
Basic data | Standard ID | SN/T 0337-2019 (SN/T0337-2019) | | Description (Translated English) | (Determination of carbofuran and its metabolite residues in foods of plant origin for export Liquid chromatography-mass spectrometry / mass spectrometry) | | Sector / Industry | Commodity Inspection Standard (Recommended) | | Classification of Chinese Standard | C53 | | Classification of International Standard | 67.050 | | Word Count Estimation | 13,120 | | Date of Issue | 2019 | | Date of Implementation | 2020-07-01 | | Issuing agency(ies) | General Administration of Customs | SN/T 0337-2019: (Determination of carbofuran and its metabolite residues in foods of plant origin for export Liquid chromatography-mass spectrometry / mass spectrometry)
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Determination of carbofuran and its metabolite residues in plant-derived food
for export --HPLC-MS/MS method
The People's Republic of China Entry-Exit Inspection and Quarantine Industry Standards
Replace SN/T 0037-.1995
Issued by the General Administration of Customs of the People's Republic of China
2019-12-27 release
2020-07-01 Implementation
Determination of carbofuran and its metabolite residues in foods of plant origin for export. Liquid chromatography-mass spectrometry/mass spectrometry
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard replaces SN 0337-95 "Test Method for Carbofuran Residues in Exported Fruits and Vegetables".
Compared with SN 0337-95, the main technical changes of this standard are as follows.
--The name of the standard was revised from "Methods for the Inspection of Carbofuran Residues in Exported Fruits and Vegetables" to "Kebufuran in Exported Plant-derived Foods"
Determination of residues of carbaryl and its metabolites by liquid chromatography-mass spectrometry/mass spectrometry"
--Increase the detection of carbofuran metabolite 3-hydroxy carbofuran;
--Expand the scope of application of standard testing;
- The sampling part has been deleted;
--Improved sample pretreatment technology;
--The instrument method was changed from gas chromatography to liquid chromatography-mass spectrometry/mass spectrometry.
--Reduce the limit of quantification, and give the recovery range of carbofuran and its metabolites for different sample matrices.
Please note that some of the contents of this document may involve patents. The issuing agency of this document is not responsible for identifying these patents.
This standard was proposed and managed by the General Administration of Customs of the People's Republic of China.
Drafting organization of this standard. China Academy of Inspection and Quarantine.
The main drafters of this standard. Li Xiaojuan, Wu Yuping, Zhang Yang, Shi Pengfei, Wang Chao, Li Shujuan.
The previous editions of the standard replaced by this standard are as follows.
Determination of carbofuran and its metabolite residues in export plant-derived foods
Liquid chromatography-mass spectrometry/mass spectrometry
1 Scope
This standard specifies the method for determining the residues of carbofuran and its metabolite 3-hydroxy carbofuran in exported plant-derived foods.
This standard applies to rice, wheat, soybean, peanut, onion, rape, spinach, tomato, cucumber, potato, orange, apple
Detection and confirmation of carbofuran and its metabolite 3-hydroxy carbofuran residues in fruits, bananas and tea.
2 Normative references
The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article
Pieces. For undated reference documents, the latest version (including all amendments) is applicable to this document.
GB/T 2763-2016 National Food Safety Standard Maximum Pesticide Residues in Food
GB/T 6682 Analytical laboratory water specifications and experimental methods
3 Principle
The sample was extracted by shaking with acidified acetonitrile, and the extract was purified by the QuEChERS method, and measured by liquid chromatography-mass spectrometry/mass spectrometry.
Determined and quantified by external standard method.
4 Reagents and materials
Unless otherwise specified, all reagents are of analytical grade, and the water is the first grade water specified in GB/T 6682.
4.1 Acetonitrile. Chromatographically pure.
4.2 Formic acid. chromatographically pure.
4.3 Acetic acid.
4.4 Sodium chloride.
4.5 Anhydrous magnesium sulfate.
4.6 Ethylenediamine-N-propyl silanized silica gel (PSA). 40 μm ～ 60 μm.
4.7 Octadecylsilane bonded silica gel (C18). 40 μm ～ 60 μm.
4.8 Graphitized carbon black (GCB). 40 μm ~ 120 μm.
4.9 0.5% acetic acid-acetonitrile solution. accurately measure 2.5 mL of acetic acid in a 500 mL volumetric flask, add acetonitrile (4.1) to constant volume, and mix well.
4.10 0.5% formic acid solution. accurately measure 2.5 mL of formic acid in a 500 mL volumetric flask, add first-grade water to the volume, and mix well.
4.11 0.1% formic acid solution. accurately measure 0.5 mL of formic acid into a 500 mL volumetric flask, add first-grade water to the volume, and mix well.
4.12 Acetonitrile-water solution (30 to 70, volume ratio). Take 30 mL of acetonitrile (4.1) and 70 mL of first-grade water and mix well.
4.13 0.1% formic acid-acetonitrile solution. accurately measure 0.5 mL of formic acid into a 500 mL volumetric flask, add acetonitrile (4.2) to a constant volume, and mix well.
4.14 Carbofuran standard substance. C12H15NO3, CAS number. 1563-66-2, purity greater than or equal to 90%.
4.15 3-hydroxy carbofuran standard product. C12H15NO4, CAS number. 16655-82-6, purity greater than or equal to 90%.
4.16 Carbofuran standard stock solution. accurately weigh 10 mg (accurate to 0.1mg) of carbofuran standard in a 10 mL volumetric flask, and use acetonitrile
(4.2) Dissolve and dilute to a constant volume, prepare a standard stock solution with a concentration of about 1 mg/mL, and store in a refrigerator at 0 ℃ ~ 4 ℃ in the dark.
4.17 3-Hydroxy carbofuran standard stock solution. accurately weigh 10 mg (accurate to 0.1mg) of carbofuran standard into a 10 mL volumetric flask, and use
Acetonitrile (4.1) is dissolved and the volume is adjusted to a standard stock solution with a concentration of about 1 mg/mL, and it is stored in a refrigerator at 0 ℃ ~ 4 ℃ in the dark.
4.18 Carbofuran standard intermediate solution. accurately draw an appropriate volume of Carbofuran standard stock solution and use acetonitrile (4.1) to prepare a concentration of 10.0
The mg/L standard intermediate solution should be stored in a refrigerator at 0℃～4℃ and protected from light.
4.19 3-hydroxy carbofuran standard intermediate solution. accurately draw an appropriate volume of 3-hydroxy carbofuran standard stock solution and prepare it with acetonitrile (4.1)
Prepare a standard intermediate solution with a concentration of 10.0 mg/L and store it in a refrigerator at 0°C to 4°C in the dark.
4.20 Carbofuran and 3-hydroxy carbofuran mixed standard working fluid. take appropriate amount of carbofuran standard intermediate solution (4.18) and 3-hydroxy carbofuran
(4.19) Standard intermediate solution, use acetonitrile-aqueous solution (4.12) to prepare a standard working solution, the working solution needs to be used on-the-spot.
5 Equipment
5.1 Liquid chromatography-mass spectrometer/mass spectrometer. equipped with electrospray ion source (ESI).
5.2 Electronic balance. Sensitivity 0.01 mg and 0.01 g.
5.3 Oscillator.
5.4 Vortex mixer.
5.5 Centrifuge. the maximum speed is not less than 10 000 r/min.
5.6 Nitrogen blowing concentrator.
5.7 High-speed centrifuge tube. specifications are 50 mL and 5 mL.
6 Sample preparation and storage
6.1 Sample preparation
Grain, oil and tea samples. take a representative sample of about 500 g, pulverize it with a grinder and pass through a 20-mesh sieve; fruits and vegetables
Vegetable samples. Take a representative sample of about 500 g, and homogenize with a homogenizer or tissue crusher. After the sample is prepared, put it into clean sample bottles
Inside, sealed and marked with a mark.
6.2 Sample storage
Samples of grains, oils and tea should be stored at 0 ℃ ~ 4 ℃; samples of fruits and vegetables should be frozen and stored below -18 ℃. Pumping
In the process of sampling and sample preparation, the samples should be prevented from being contaminated or from changing the content of residues.
7 Measurement procedure
7.1 Extraction
7.1.1 Vegetables and fruits. Weigh 5 g sample (accurate to 0.01 g) into a 50 mL centrifuge tube, add 10 mL 0.5% acetic acid-acetonitrile solution
Solution (4.9), vortex and mix well, shake and extract for 30 minutes, add about 2 g sodium chloride and about 2 g anhydrous magnesium sulfate, vortex and mix, 20 000 r/min
Centrifuge under conditions for 3 min, and take the supernatant for purification.
7.1.2 Grains, oils and teas. Weigh 2 g sample (accurate to 0.01 g) into a 50 mL centrifuge tube, and add 5 mL 0.5% acetic acid to dissolve it.
Solution (4.10), vortex and mix and let stand for 30 min, add 10 mL of 0.5% acetic acid-acetonitrile solution (4.9), vortex and mix, shake and extract for 30 min.
Add about 2 g of sodium chloride and about 2 g of anhydrous magnesium sulfate, vortex to mix, centrifuge at 10 000 r/min for 3 min, and take the supernatant for purification.
7.2 Purification
Accurately weigh 250 mg anhydrous magnesium sulfate, 100 mg PSA, 100 mg C18 and 50 mg GCB purification material and add 5 mL high speed
SN/T 0037-2019
Centrifuge tube. Accurately pipet 2mL supernatant (7.1) into a 5mL high-speed centrifuge tube, vortex to mix, and centrifuge at 10 000 r/min
3 min, take 1 mL of supernatant and place it in a glass tube, blow nitrogen to near dryness at 40 ℃, and then add 1.0 mL of acetonitrile-aqueous solution (4.12)
Fully dissolve in a constant volume, pass through a 0.2 μm nylon filter membrane, and wait for LC-MS/MS determination.
7.3 Liquid chromatography-mass spectrometry/mass spectrometry
7.3.1 Liquid chromatography conditions
7.3.1.1 Chromatographic column. C18, 100 mm × 2.1 mm × 1.7 μm, or equivalent performance.
7.3.1.2 Column temperature. 45 ℃.
7.3.1.3 Injection volume. 5 μL.
7.3.1.4 The mobile phase and gradient elution conditions are shown in Table 1.
7.3.2 Mass spectrometry conditions
For instrument mass spectrometry conditions, see Appendix A.
7.3.3 Qualitative determination
Determine the standard solution and sample solution according to the conditions in 7.3.1, if the difference between the retention time of the sample solution and the standard solution's mass chromatographic peak does not exceed
±2.5%, in the mass spectrum after subtracting the background, all the selected monitoring ions appear, and the relative abundance of the qualitative ion (using relative
It is expressed as a percentage of the intensity of the strongest ion abundance) and the relative abundance of the standard working solution with the same concentration is consistent...
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