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GB 23200.6-2016 English PDF

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GB 23200.6-2016: Food safety national standard -- Methods for the determination of herbicide residues -- Part 6: Determination of herbicidal residues in food by liquid chromatography-mass spectrometry / mass spectrometry
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GB 23200.6-2016English259 Add to Cart 3 days [Need to translate] Food safety national standard -- Methods for the determination of herbicide residues -- Part 6: Determination of herbicidal residues in food by liquid chromatography-mass spectrometry / mass spectrometry Valid GB 23200.6-2016

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Basic data

Standard ID GB 23200.6-2016 (GB23200.6-2016)
Description (Translated English) Food safety national standard -- Methods for the determination of herbicide residues -- Part 6: Determination of herbicidal residues in food by liquid chromatography-mass spectrometry / mass spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 13,132
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 1737.6-2010
Regulation (derived from) State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of 2016
Issuing agency(ies) National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration

GB 23200.6-2016: Food safety national standard -- Methods for the determination of herbicide residues -- Part 6: Determination of herbicidal residues in food by liquid chromatography-mass spectrometry / mass spectrometry



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Food safety national standard - Methods for the determination of herbicide residues - Part 6. Determination of herbicidal residues in food by liquid chromatography - mass spectrometry/mass spectrometry National Standards of People's Republic of China GB Replace SN 1737.6-2010 National standards for food safety Method for determination of herbicide residue Part 6. Determination by liquid chromatography - mass spectrometry/mass spectrometry The amount of herbicides in the food National food safety standards- Determination of amitrole residue in foods Liquid chromatography - mass spectrometry 2016-12-18 Release.2017-06-18 Implementation National Health and Family Planning Commission of the People 's Republic of China Issued by the Ministry of Agriculture of the People 's Republic of China State Administration of Food and Drug Administration

Foreword

This standard replaces SN 1737.6-2010 "Liquid Chromatography-Mass Spectrometry/Mass Spectrometry" for the detection of herbicidal residues in foodstuffs for import and export. This standard compared with SN 1737.6-2010, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - the name of the "import and export food" to "food"; - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN 1737.6-2010. National standards for food safety Method for determination of herbicide residue Part 6. Determination of herbicidal residues in food by liquid chromatography - mass spectrometry/mass spectrometry

1 Scope

This standard specifies the method of LC-MS-MS for the determination of herbicidal residues in foodstuffs by liquid chromatography-tandem mass spectrometry (LC-MS-MS). This standard applies to apples, pineapples, spinach, carrots, basil leaves, honeysuckle, ginger powder, pepper powder, tea, wheat, corn, Peanut, meat, fish and animal liver in the killing of grass strong residue detection and confirmation; other food can refer to the implementation.

2 normative reference documents

The following documents are indispensable for the application of this document. For dated references, only the dated edition applies to this article Pieces. For undated references, the latest edition (including all modifications) applies to this document. GB 2763 National Standard for Food Safety - Maximum Residue Limit of Pesticides in Foodstuffs GB/T 6682 Analytical laboratory water specifications and test methods

3 principle

The samples were extracted and purified by PCX solid phase extraction column or ENVI-Carb solid phase extraction column. Liquid chromatography-mass spectrometry/mass spectrometry Quantitative quantity.

4 reagents and materials

Unless otherwise specified, all reagents are chromatographic pure, water to meet the GB/T 6682 in the provisions of a water. 4.1 Reagents 4.1.1 glacial acetic acid (C2H4O2). 4.1.2 Ammonia (NH4OH). 4.1.3 Dichloromethane (CH2Cl2). 4.1.4 Acetone (C3H6O). 4.2 solution preparation 4.2.1 1% acetic acid solution. absorb 10 mL of glacial acetic acid, with ultra-pure water volume to 1 L. 4.2.2 25% acetone - water solution. the amount of 250 mL of acetone, with ultra-pure water volume to 1 L. 4.2.3 1% acetic acid - acetone - water solution. absorb 10 mL of glacial acetic acid, with acetone aqueous solution to 1 L. 4.2.4 5% ammoniated methanol solution. absorb 5 mL of ammonia, with methanol volume to 100 mL. 4.3 standards 4.3.1 Straw standard material. Amitrole, C2H4N4, molecular weight. 84.08, CAS. 61-82-5, purity ≥ 99.9%. 4.4 standard solution preparation 4.4.1 to kill grass strong standard stock solution. Weigh the appropriate amount of saccharification standard (accurate to 0.1mg) in 50mL volumetric flask, with acetonitrile prepared into 1.0 Mg/mL standard stock solution; 0 ~ 4 0C preservation. 4.4.2 to kill grass strong standard working fluid. according to the need for mobile phase diluted with the preparation of the preparation of the standard concentration of the standard working fluid. 0-4 0C Save 4.5 Materials 4.5.1 PCX solid phase extraction column. 60 mg/3 mL or equivalent. (Mixed cation exchange column). 4.5.2 ENVI-Carb solid phase extraction column. 500 mg/6 mL or equivalent, (graphitized non-porous carbon). 4.5.3 Filtration. 0.2 μm.

5 instruments and equipment

5.1 Liquid Chromatography-Mass Spectrometry/Mass Spectrometer. Equipped with an electrospray ion source (ESI). 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 whirlpool mixer. 5.4 Rotary Evaporator. 5.5 high speed homogenizer. 5.6 Centrifuge. 5.7 Oscillator. 5.8 Grain grinder. 5.9 Food muffler. 5.10 peanut grinder. 5.11 centrifuge tube. 100 mL, 50 mL. 5.12 capacity bottle. 100 mL.

6 Preparation and storage of samples

6.1 Preparation of the sample 6.1.1 wheat, corn, honeysuckle, tea Approximately 500 g of representative sample, crushed with a pulverizer and passed through a 2.0 mm round hole screen. Mix well, into a clean container, Sealed, marked. 6.1.2 fruits, vegetables, fish, meat, liver Approximately 500 g of representative sample was taken and the sample was processed into a slurry with a food masher. Mix well, into a clean container, Sealed, marked. 6.1.3 ginger powder, pepper powder Take a representative sample of about 100 g, fully mixed evenly, over 2.0 mm round hole sieve, into a clean container, sealed, marked mark. 6.1.4 peanuts Take a representative sample 500 g, all grinding with an attritor. Mix well, into a clean container, sealed, marked mark. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 6.2 Sample storage Wheat, corn, peanuts, tea, ginger powder, pepper powder samples stored at 0-4 ℃; fish, meat, liver and fruit and vegetable samples Frozen at -18 ° C or lower. During sample and sample preparation, the sample should be protected from contamination or changes in the residue content.

7 Analysis steps

7.1 Extraction 7.1.1 apple, pineapple, spinach, carrot, basil leaves Weigh 10 g of sample (accurate to 0.1 g) in a 100 mL centrifuge tube, add 20 Ml of 1% acetic acid solution and 20 mL of dichloromethane,.20000 R/min homogeneous 1 min, centrifuged at 5000 r/min 5 min, supernatant into 100 mL volumetric flask, discard the lower layer of methylene chloride, residue With 1% acetic acid solution 20 mL and dichloromethane 20 mL repeated extraction time; combined supernatant, with 1% acetic acid solution to the scale, remove 10 ML of the extract to be purified. 7.1.2 honeysuckle, ginger powder, pepper powder, tea leaves Weigh 1 g sample (accurate to 0.01 g) in 50 mL centrifuge tube, add 20 mL 1% acetic acid aqueous solution,.20000 r/min homogeneous 1 min, 5000 r/min centrifugal 5 min, the supernatant filtered into the 125 mL separatory funnel, the residue and then 10 mL 1% acetic acid aqueous solution repeated extraction time, The supernatant was combined, 10 mL of dichloromethane was added, shaken for 1 min, left to stand, and the lower layer of methylene chloride was discarded. To be purified. 7.1.3 corn, peanuts Weigh 2 g sample (accurate to 0.01 g) in 50 mL centrifuge tube, add 20 mL 1% acetic acid-acetone aqueous solution,.20000 r/min 1 min, 5000 r/min centrifugation 5 min, the supernatant filter filter to 125 mL separatory funnel, the residue and then 10 mL 1% acetic acid - acetone The aqueous solution was repeated once, the supernatant was added, 10 mL of methylene chloride was added, shaken for 1 min, and the layers were separated and the lower layer of methylene chloride was discarded. To be purified. 7.1.4 Wheat, fish, meat, liver Wheat, fish, meat, weighed 2 g sample, the liver weighed 1 g sample (accurate to 0.01 g) in 50 mL centrifuge tube, add 20 mL of acetone Aqueous solution,.20000 r/min homogeneous 1 min, 5000 r/min centrifugation 5 min, the extract was filtered to 125 mL separatory funnel, the residue with 10 ML aqueous solution of acetone was repeated once, the supernatant was added, 10 mL of methylene chloride was added, shaken for 1 min, and the layers were separated and discarded. Methane layer. The solution was added with 0.25 mL of glacial acetic acid to be purified. 7.2 Purification 7.2.1 apple, pineapple, spinach, carrot, basil leaves, corn, peanuts, wheat, fish, meat, liver The PCX cartridge was pre-eluted with 3 mL of methanol and 5 mL of water, and the effluent was discarded. Inject the extract, then 3 mL of water, 3 mL of methanol Rinse and discard the effluent. The eluent was eluted with 2 mL of 5% ammoniated methanol solution and concentrated at 40 ° C to near dryness. The residue was washed with 1.0 mL The mobile phase was dissolved and passed through a 0.2 μm membrane for liquid chromatography - mass spectrometry/mass spectrometry. 7.2.2 honeysuckle, ginger powder, pepper powder, tea Envi-Carb was pre-eluted with 3 mL of methanol and 3 mL of water. The effluent was discarded and the extract was filled and the effluent was collected. The PCX cartridge was pre-eluted with 3 mL of methanol and 5 mL of water, and the effluent was discarded. The Envi-Carb purified sample was transferred to a PCX purification column, And then with 3 mL of water, 3 mL of methanol leaching, with 2 mL 5% ammoniated methanol solution elution, the eluent collected at 40 ° C concentrated to near dry, The residue was dissolved in 1.0 mL mobile phase and passed through a 0.2 μm filter for liquid chromatography-mass spectrometry/mass spectrometry. 7.3 Determination 7.3.1 Liquid Chromatography - Mass Spectrometry/Mass Spectrometry Reference Conditions A. Column. CAPCELL PAK (1. 4) 2.00mmI.D. * 100mm 5μm or equivalent B. Mobile phase. 10 mmol acetic acid amine, 0.1% formic acid water PH = 3 (A) acetonitrile (B) Table 1 Mobile phase conditions Condition Sample name Flow rate/mL/min% A% B Condition 1 fish, meat, ginger, pepper, liver, tea 0.20 20 80 Condition 2 apple, pineapple, spinach, carrot, Basil leaves, honeysuckle, wheat, corn, peanut 0.20 50 50 C. Column temperature. 40 ° C. D. Flow rate. 0.2 mL/min. E. Injection volume. 10 μL. F. Mass spectrometry conditions. see Appendix A, A.1 7.3.2 Determination and confirmation of chromatography According to the sample content of the sample, the selected concentration of similar standard working solution, the standard working solution and sample solution volume into the sample The response values of dinduazites in the standard working solution and the sample to be tested shall be within the linear range of the instrument. If the sample solution is in the mass chromatogram of the standard working solution, the chromatographic peaks appear at the same retention time, the allowable deviation is less than ± 2.5% The abundance ratio of the selected ions is greater than the abundance ratio of the corresponding ions of the standard, and the value is within the allowable range (see Table 2). You can judge the sample There is a corresponding test object in the product. In the case of 6.3.1, the liquid chromatography-mass spectrum of the herbicidal standard is shown in Appendix B. Table 2 Use Qualitative Liquid Chromatography - Mass Spectrometry Relative Ion Abundance Maximum Allowable Deviation Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10% Allowable relative deviation ± 20% ± 25% ± 30% ± 50% 7.4 blank experiment In addition to the sample, according to the above determination steps.

8 results are calculated and expressed

Use the chromatographic data processor or according to formula (1) to calculate the amount of saccharide residues in the sample. A × c × V AS x m (1) Where. X - the amount of residue in the sample, in milligrams per kilogram (μg/kg); A - the peak area of the herbicide in the sample solution; The concentration of the working fluid is in micrograms per milliliter (μg/L). V - the final volume of the sample solution in milliliters (mL); AS - the peak area of standard working solution; M - the final sample quality of the sample, in units of (g). Note. The result of the calculation shall be deducted from the blank value. The result of the measurement shall be expressed as the arithmetic mean of the parallel measurement, and two valid digits shall be retained.

9 precision

9.1 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with Appendix D requirements. 9.2 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with Appendix E requirements. 10% limit and recovery rate 10.1 Quantitation limits The limit of quantification for apple, pineapple, spinach, carrot, basil leaves, corn, peanuts, wheat, ginger, fish, meat and liver is 0.01mg/kg, in tea, honeysuckle, pepper quantitative limit of 0.02 mg/kg. 10.2 Recovery rate The experimental data on the concentration and recovery of the sample are given in Appendix C.

Appendix A

Table A.1 Mass spectrometry conditions Table A.2 Multi-reaction monitoring conditions Note. Add "*" ions for quantitation. Non-Commercial Notices. The parameters listed in Appendix A are performed on an Agilent 6410A mass spectrometer, where the test instrument is listed for Provide reference, does not involve commercial purposes, to encourage standard users to try to use different manufacturers or models of equipment. Ionization mode ESI Electrospray voltage 4000V The source temperature is 350 ° C Atomizer pressure nitrogen, 40 psi Dry gas nitrogen, flow rate 10L/min Solvent gas stream nitrogen, 600 L/h Collision air pressure, 3.10 × 10-6 Pa Monitoring mode multiple reaction monitoring Compound ion ion ion residence time cone hole voltage collision energy Kill grass strong 85 43 * 0.20 s 100 V 25 eV 57 0.20 s 100 V 15eV

Appendix B

Standard substance chromatogram Figure B.1 Table 1 conditions 1 under the grass strong liquid chromatography - mass spectrometry/mass spectrometry multi-reaction monitoring chromatogram Figure B.2 Table 1 under the conditions of 2 under the grass strong liquid chromatography - mass spectrometry/mass spectrometry multi-reaction monitoring chromatogram 0.08 mg/L standard

Appendix C

(Informative) Sample concentration and recovery of the experimental data Table C.1 Experimental data on the concentration and recovery of the sample sample name Add concentration (Μg/kg) Recovery rate(%) peanut 10 62.50 to 72.00 20 67.00 ~ 80.00 40 75.75 ~ 85.00 corn 10 61.00 ~ 78.00 20 74.50 to 84.30 40 79.20 ~ 88.00 wheat 10 69.50 to 85.70 20 78.45 ~ 90.00 40 76.00 ~ 93.50 Basil 10 79.22 ~ 82.60 20 71.50 to 91.00 40 85.32 ~ 91.10 pork 10 66.70 ~ 73.20 20 68.40 ~ 81.10 40 78.50 to 85.40 spinach 10 87.20 ~ 98.20 20 90.04 ~ 103.23 40 89.54 ~ 98.55 Salmon 10 69.00 ~ 78.00 20 76.50 to 85.20 40 75.00 ~ 87.50 apple 10 78.40 ~ 83.30 20 77.90 ~ 90.90 40 82.05 to 92.41 Pepper 20 75.00 ~ 94.65 40 81.97 ~ 90.92 80 83.82 ~ 88.99 10 62.80 to 85.60 20 80.30 ~ 82.80 40 80.61 ~ 86.69 honeysuckle 20 69.80 to 88.30 40 81.90 ~ 89.00 80 80.49 ~ 85.40 carrot 10 68.40 ~ 78.50 20 74.50 to 85.45 40 79.20 ~ 94.20 pineapple 10 63.80 to 77.10 20 81.20 to 86.50 40 85.21 ~ 98.52 tea 20 63.25 ~ 79.36 40 71.31 ~ 78.63 80 80.65 ~ 88.63 liver 10 71.31 ~ 78.63 20 70.87 to 81.07 40 81.31 ~ 88.63

Appendix D

(Normative appendix) Laboratory repeatability requirements Table D.1 Laboratory repeatability requirements Measured component content Mg/kg Precision 0.001 36 > 0.01 > 1 14

Appendix E

(Normative appendix) Inter-laboratory reproducibility requirements Table E.1 Inter-laboratory reproducibility requirements Measured component content Mg/kg Precision 0.001 54 > 0.01 > 1 19

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