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GB 31658.10-2021: National food safety standard - Determination of carbamate insecticides residues in animal derived foods by liquid chromatography-tandem mass spectrometry method
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National food safety standard - Determination of carbamate insecticides residues in animal derived foods by liquid chromatography-tandem mass spectrometry method
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GB 31658.10-2021
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Basic data | Standard ID | GB 31658.10-2021 (GB31658.10-2021) | | Description (Translated English) | National food safety standard - Determination of carbamate insecticides residues in animal derived foods by liquid chromatography-tandem mass spectrometry method | | Sector / Industry | National Standard | | Classification of Chinese Standard | X04 | | Word Count Estimation | 9,997 | | Issuing agency(ies) | National Health Commission of the People's Republic of China, State Administration for Market Regulation | GB 31658.10-2021: National food safety standard - Determination of carbamate insecticides residues in animal derived foods by liquid chromatography-tandem mass spectrometry method
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National food safety standards
Carbamate pesticides in animal foods
Determination of residual amounts liquid chromatography-tandem mass spectrometry
National Standards of People's Republic of China
Released by the National Health Commission of the People's Republic of China
State Administration for Market Regulation
Ministry of Agriculture and Rural Affairs of the People's Republic of China
Foreword
This document complies with the provisions of GB/T 1:1-2020 "Standardization Work Guidelines Part 1: Structure and Drafting Rules of Standardization Documents"
Drafting:
1 Scope
This document specifies the carbamate pesticides (carbofuran, 3-hydroxycarbofuran, aldicarb, aldicarb, etc:) in pig, cattle, sheep, chicken tissues (muscle, liver, kidney and fat), eggs and milk: Methiocarb sulfone, aldicarb sulfoxide, methomyl, methiocarb, methiocarb, methiocarb, methiocarb, methiocarb sulfone, methiocarb sulfoxide, pirimicarb, desmethylmethiocarb Sample preparation and liquid chromatography-tandem mass spectrometry method for detection of residues of ethylcarb, ethiobencarb, isoprocarb, carbaryl, dipiocarb, propoxur, secbutylcarb, fenoxycarb, and indoxacarb:
This document is applicable to the determination of carbamate pesticide residues in pig, cattle, sheep, chicken tissues (muscle, liver, kidney and fat), eggs and milk:
2Normative reference documents
The contents of the following documents constitute essential provisions of this document through normative references in the text: Among them, for dated reference documents, only the version corresponding to the date applies to this document; for undated reference documents, the latest version (including all amendments) applies to this document:
GB/T 6682 Specifications and test methods for water used in analytical laboratories
3Terms and Definitions
There are no terms or definitions to be defined in this document:
4 Principles
The target compound remaining in the sample was extracted with acetonitrile, degreased with n-hexane, enriched and purified by solid-phase extraction, measured by liquid chromatography-tandem mass spectrometry, and quantified by the external standard method:
5Reagents and materials
Unless otherwise specified, all reagents are of analytical grade and the water is first-grade water that complies with GB/T 6682:
5:1 Reagents
5:1:1 Acetonitrile (CH₃CN): chromatographically pure:
5:1:2 Methanol (CH₂OH):
5:1:3 Formic acid (HCOOH): chromatographically pure:
5:1:4 n-hexane (C, Hμ)
5:1:5 Dichloromethane (CH₂Cl₂):
5:1:6 Sodium chloride (NaCl),
5:1:7 Anhydrous sodium sulfate (Na₂SO₄):
5:2 Solution preparation
5:2:1 Dichloromethane-methanol solution: Take 99 mL of dichloromethane and 1 mL of methanol, and mix well:
5:2:2 25% acetonitrile solution: Take 25 mL of acetonitrile and 75 mL of water, and mix well:
5:2:30:1% formic acid solution: Take 1mL of formic acid, dilute it with water to 1000mL, and mix well:
5:2:4 Saturated sodium chloride solution: Take 50g of sodium chloride, add 100mL of water, shake while adding, and let stand:
5:3 Standard products: carbofuran, 3-hydroxycarbofuran, aldicarb, aldicarb sulfone, aldicarb sulfoxide, methomyl, methiocarb, methiocarb, methiocarb, methiocarb, methiocarb Dimethiocarb sulfone, dipiocarb sulfoxide, pirimicarb, desmethylpipicarb, ethiobencarb, isoprocarb, carbaryl, dipiocarb, propoxur, butylcarb, fenoxycarb and indene Chongiocarb, the content is ≥95%, see Appendix A:
5:4 Preparation of standard solution
5:4:1 Standard stock solution: Take about 10 mg of each carbamate pesticide standard, weigh it accurately, add an appropriate amount of acetonitrile to dissolve and dilute to a 10 mL brown volumetric flask, and prepare a solution with a concentration of 1000 μg/mL: Standard stock solution: Store in a dark place below -18℃, valid for 6 months:
5:4:2 Mixed standard intermediate solution: Accurately pipette 1 mL of each standard stock solution into a 100 mL brown volumetric flask, dilute to the mark with acetonitrile, and prepare a mixed standard intermediate solution with a concentration of 10 μg/mL: Store in a dark place below -18℃, valid for 6 months:
5:4:3 Mixed standard working solution: Accurately pipet an appropriate amount of the mixed standard intermediate solution, and dilute it with 25% acetonitrile solution to a concentration of 2 μg/L, 5 μg/L, 20 μg/L, 50 μg/L,:200 μg/L and 500 μg/L: L series mixed standard working fluid: Ready for use:
5:5 Materials
5:5:1 Amino solid-phase extraction column: 500 mg/6mL, or equivalent, activated with 4mL of dichloromethane-methanol solution before use:
5:5:2 Syringe filter (universal filter membrane): pore size 0:22μm, organic system:
6Instruments and equipment
6:1 Liquid chromatography tandem mass spectrometer: equipped with electrospray ion source:
6:2 Analytical balance: sensitive to 0:01g and 0:00001g:
6:3 Nitrogen blowing instrument:
6:4 Solid phase extraction device:
6:5 Centrifuge tube: polypropylene plastic centrifuge tube, 50 mL:
6:6 Centrifuge: 5000 r/min or above:
6:7 Vortex mixer:
7 Preparation and preservation of samples
7:1 Preparation of samples
Take an appropriate amount of fresh or thawed blank or test tissue, mince it, and homogenize it:
a) Take the homogenized test sample as the test material;
b) Take the homogenized blank sample as the blank sample;
c) Take the homogenized blank sample, add the standard working solution of appropriate concentration, and add the sample as a blank:
7:2 Storage of samples
Store below -18℃ and conduct analysis and testing within 3 months:
8 Measurement steps
8:1 Extraction
Take 5g of the sample (accurate to ±0:05g), put it in a 50mL plastic centrifuge tube, add 5g of anhydrous sodium sulfate and 15 mL of acetonitrile in sequence, vortex for 1 min, shake for 30 min, centrifuge at 5000 r/min for 5 min, and collect the supernatant solution, add 10 mL of acetonitrile to the residue, repeat the extraction once, combine the extracts, and set aside:
8:2 Purification
Take the reserve solution, add 10 mL of saturated sodium chloride solution and 10 mL of n-hexane, vortex for 1 min, and centrifuge at 5000 r/min for 3 min: Take the acetonitrile solution of the middle layer in a 50 mL plastic centrifuge tube, and blow with nitrogen in a 40°C water bath until it is nearly dry: Add 2 mL of dichloromethane-methanol solution to dissolve the residue, pass it through the activated amino solid-phase extraction column, collect the effluent, wash the 50 mL plastic centrifuge tube with 2 mL of dichloromethane-methanol solution, and pass through the column: Repeat once to collect all the effluent: liquid, blow with nitrogen in a 50°C water bath until it is nearly dry, dissolve the residue with 1:0 mL of 25% acetonitrile solution, vortex to mix, and filter with a 0:22 μm filter membrane for liquid chromatography-tandem mass spectrometry measurement:
8:3 Preparation of standard curve
Take a series of mixed standard working solutions of 2 μg/L, 5 μg/L, 20 pg/L, 50 pg/L,:200 pg/L and 500 μg/L, and inject samples for liquid chromatography-tandem mass spectrometry measurement: Using the quantitative ion pair peak area as the ordinate and the standard solution concentration as the abscissa, draw a standard curve and find the regression equation and correlation coefficient:
8:4 Determination
8:4:1 Liquid Chromatography Reference Conditions
a) Chromatographic column: Cis column (100 mm×2:1mm, 1:7μm), or equivalent;
b) Mobile phase: A is 0:1% formic acid solution, B is acetonitrile, gradient elution conditions are shown in Table 1; c) Flow rate: 0:3mL/min;
d) Column temperature: 35℃;
e) Injection volume: 10 μL:
8:4:2 Mass spectrometry reference conditions
a) Ion source: electrospray ion source;
b) Scanning method: positive ion scanning;
c) Detection method: multiple reaction monitoring (MRM);
d) Capillary voltage: 2:5kV;
e) RF lens voltage: 0:5V;
f) Ion source temperature: 150℃;
g) Desolvation gas temperature: 600℃;
h) Cone air flow rate: 50 L/h;
i) Desolvation gas flow rate: 1000 L/h;
j) Multiplier voltage: 650 V;
k) Secondary collision gas: argon; 8:4:3 Determination method
Take the sample solution and the mixed standard solution for single-point or multi-point calibration, and use the chromatographic peak area for quantification according to the external standard method: The response value of the analyte in the sample solution should be within the linear range of the instrument measurement: The retention time of the substance to be measured in the sample is different from the retention time of the substance to be measured in the standard solution:
If the difference is within ±2:5%, and the relative ion abundance of each component in the sample is consistent with the relative ion abundance of the standard solution with a similar concentration, and the deviation does not exceed the range specified in Table 3, it can be determined that the corresponding component exists in the sample: Analyte: See Appendix B for the multiple reaction monitoring chromatogram of the standard working solution: 8:5 Blank test
Take a blank sample and perform parallel operations using the same measurement steps except that no standard solution is added:
9Result calculation and presentation
The residual amount of the substance to be tested in the sample is calculated according to the standard curve or formula (1): 10 Sensitivity, accuracy and precision of detection methods
10:1 Sensitivity
The detection limit of this method in pig, cattle, sheep, chicken tissues (muscle, liver, kidney and fat), eggs and milk is 0:5μg/kg, and the quantitation limit is
is 1:0pg/kg:
10:2 Accuracy
The recovery rate of this method at the added concentration level of 1 μg/kg to 5 μg/kg is 60% to 110%:
10:3 Precision
The intra-batch relative standard deviation of this method is ≤15%, and the inter-batch relative standard deviation is ≤20%:
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