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GB 23200.63-2016 English PDF

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GB 23200.63-2016: Food safety national standard -- Determination of thiazolylamine residues in food by liquid chromatography-mass spectrometry / mass spectrometry
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GB 23200.63-2016English239 Add to Cart 3 days [Need to translate] Food safety national standard -- Determination of thiazolylamine residues in food by liquid chromatography-mass spectrometry / mass spectrometry Valid GB 23200.63-2016

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Basic data

Standard ID GB 23200.63-2016 (GB23200.63-2016)
Description (Translated English) Food safety national standard -- Determination of thiazolylamine residues in food by liquid chromatography-mass spectrometry / mass spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 12,159
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 2514-2010
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 23200.63-2016: Food safety national standard -- Determination of thiazolylamine residues in food by liquid chromatography-mass spectrometry / mass spectrometry


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Food safety national standard - Determination of thiazolylamine residues in food by liquid chromatography - mass spectrometry/mass spectrometry National Standard of the People 's Republic of China GB Replace SN/T 2514-2010 National standards for food safety Determination of thiazolylamine residues in food Liquid chromatography - mass spectrometry/mass spectrometry National food safety standards- Determination of tiadinil 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/T 2514-2010 "Determination of thiazolylamine pesticide residues in import and export food by liquid chromatography-mass spectrometry". Compared with SN/T 2514-2010, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - the name and scope 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/T 2514-2010. National standards for food safety Determination of thiazolylamine pesticide residues in food by liquid chromatography - mass spectrometry/mass spectrometry

1 Scope

This standard specifies the method of liquid chromatography-mass spectrometry/mass spectrometry for the determination of thiazolylamine pesticide residues in food. This standard applies to lettuce, carrots, cabbage, rice, citrus, grapes, chestnut, beef, sheep liver, chicken, tilapia, fan Eggplant, tea, honey, thiadiazole pesticide residues in the qualitative identification/quantitative determination of 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 with ethyl acetate, gel chromatographed (GPC) and solid phase extraction (SPE), and identified by liquid chromatography-mass spectrometry/mass spectrometry. External standard method.

4 reagents and materials

Unless otherwise specified, all reagents are of analytical grade and water is in accordance with the primary water specified in GB/T 6682. 4.1 Reagents 4.1.1 Cyclohexane (C6H12,110-82-7). Chromatographic Purification. 4.1.2 Ethyl acetate (C4H8O2,141-78-6). Chromatographic pure. 4.1.3 acetonitrile (C2H3N, 75-05-8). pure chromatography. 4.1.4 Methanol (CH4O, 67-56-1)). Chromatographic pure. 4.1.5 anhydrous sodium sulfate (Na2SO4,15124-09-1). 650 ℃ burning 4 h, in the dryer to cool to room temperature, stored in a sealed bottle spare. 4.1.6 Sodium chloride (NaCl, 7647-14-5). 4.2 standards 4.2.1 tiadinil standard (C11H10ClN3OS, CAS. 223580-51-6). purity ≥ 97.0%. 4.3 standard solution preparation 4.3.1 Thiamidylamine Pesticide Standard stock solution. accurately weighed the appropriate amount of thiadiazole pesticide standard substance, with acetonitrile prepared into a concentration of 1.0 Mg/mL standard stock solution. 4.3.2 Thiamidylamine Standard Intermediate Solution. Accurately absorb the appropriate amount of standard stock solution, diluted with acetonitrile to a concentration of 10.0 ug/mL Inter-solution. 4.3.3 Thiamidose standard working solution. Before use, the standard intermediate solution is diluted with a blank matrix of various samples to the appropriate concentration Of the standard working fluid. 4.4 Materials 4.4.1 Amino solid phase extraction column..200 mg, 3 mL and 500 mg, 3 mL, or equivalent. Before use, use acetonitrile to the amino column (200 Mg) was activated twice a day for 2 mL. In the amino column (500 mg) filled with 0.5 g anhydrous sodium sulfate, before use with ethyl acetate activated 2 times, Each time 2 mL. 4.4.2 CHROMABOND XTR Solid phase extraction column (large pore diatomaceous earth filler). 3000 mg, 15 mL, or equivalent. 4.4.3 Microporous membrane. 0.2 μm and 0.45 μm, organic phase.

5 instruments and equipment

5.1 Liquid Chromatography-Mass Spectrometry/Mass Spectrometer. Equipped with electrospray ion source. 5.2 Gel Permeation Chromatography. 5.3 Analysis of balance. 0.01 g and 0.0001 g. 5.4 high-speed homogenizer. 5.5 high-speed low-temperature refrigerated centrifuge. 10000 r/min. 5.6 Rotary Evaporator. 5.7 nitrogen dryers. 5.8 Swirl Oscillator. 5.9 Polytetrafluoroethylene plastic centrifuge tube. 50 mL, with plug. 5.10 glass scale test tube, 5 mL and 10 mL, with plug. 5.11 heart bottle. 50 mL.

6 Preparation and storage of samples

6.1 Preparation of the sample 6.1.1 lettuce, carrots, cabbage, citrus, grapes Take a representative sample of about 500 g, chopped it, and processed into a slurry with a mashed machine. Mix well, fit into clean container, seal, mark mark. 6.1.2 rice, chestnut, tea Approximately 500 g of representative sample was pulverized and pulverized through a pulverizer and passed through a 1.2 mm round hole. Mix, mix into a clean container, Mark the mark. 6.1.3 beef, chicken, sheep liver, tilapia Take a representative sample of about 500 g, minced with a meat grinder, mix well, into a clean container, sealed, marked mark. 6.1.4 tomato sauce Take a representative sample of about 500 g, mix, mix into a clean container, seal, mark the mark. 6.1.5 honey To replace the sample of about 500 g, the crystallization of honey samples will be evenly stirred; on the crystallization of honey samples, in a closed situation Conditions, the sample bottle placed in not more than 60 ℃ in the water bath in the warm, shaking, until the sample all melt and stir well, quickly cooled to room temperature, In the melting must pay attention to prevent moisture evaporation. Load a clean container, seal, mark the mark. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 6.2 Sample storage Tea, honey, grain and nuts and other samples stored at 0 ~ 4 ℃; fruits and vegetables and animal-derived food samples at -18 ℃ to Frozen under the preservation. 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 lettuce, carrots, cabbage, citrus, grapes, chestnuts, beef, sheep liver, chicken, tilapia, tomato sauce Weigh 10 g (accurate to 0.01 g) sample in 50 mL centrifuge tube, add 15.0 mL ethyl acetate, homogeneous extraction 1 min, another A 50 mL centrifuge tube, add 10.0 mL of ethyl acetate to wash the homogenizer tip, merge the homogeneous solution. Add 10 g of anhydrous sodium sulfate, shake 10 min. Extract 10 r/min centrifugal 5 min, draw 10.0 mL supernatant, the refrigerator below 0 ℃ placed 10 h, over 0.45 μm Machine filter, to be gel permeation chromatography purification. 7.1.2 Rice Weigh 10 g (accurate to 0.01 g) sample in a 50 mL centrifuge tube, add 10.0 mL of water, soak for 20 min, add 15.0 mL B Ethyl acetate, homogeneous extraction 1 min, another take a 50 mL centrifuge tube, add 10.0 mL of ethyl acetate wash homogenizer head, combined homogeneous solution. Add 10 g of anhydrous sodium sulfate, shake 10 min. The sample extract was centrifuged at 10000 r/min for 5 min, and 10.0 mL supernatant was taken Box below 0 ℃ for 10 h, then 0.45 μm organic filter, to be gel permeation chromatography purification. 7.1.3 Tea Weigh 2 g (accurate to 0.01 g) sample in a 50 mL centrifuge tube, add 10.0 mL of water, soak for 20 min, add 1 g Water sodium sulfate, vortex oscillation 1 min. Add 10.0 mL of ethyl acetate, vortex for 2 min, centrifuge the sample extract at 4000 r/min Min, learn supernatant. Then add 10.0 mL of ethyl acetate, vortex oscillation 2 min, 4000 r/min centrifugation 5 min, repeated extraction time, Combined with the supernatant, 45 ℃ blowing nitrogen concentrated to about 2 mL, constant volume to 10 mL, over 0.45 μm organic filter, to be gel permeation color Spectrum purification. 7.1.4 honey Weigh 2.0 g (accurate to 0.01 g) sample in 50 mL centrifuge tube, add 3 mL of water, 0.5 g sodium chloride, shock mix, over XTR Solid phase extraction column. After loading, the sample solution was kept for 5 min, eluted with 35 mL of ethyl acetate several times, the flow rate was 1.0 mL/min, The filtrate was collected in a 50 mL chicken heart and concentrated under reduced pressure at 45 ° C to about 0.5 mL to be purified. 7.2 Purification 7.2.1 lettuce, carrots, cabbage, citrus, grapes, chestnut, beef, sheep liver, chicken, tilapia, tomato sauce, rice, tea 10 mL of the obtained solution of 7.1.1, 7.1.2 and 7.1.3, and the supergel permeation chromatography was used to collect the effluent from 7 to 14 min. Shrink the device, concentrated at 45 ℃ to near dry, 2 mL acetonitrile volume, as the initial purification solution. After the primary cleaning solution was passed through the amino column (200 mg), the flask was washed three times with acetonitrile, 1 mL each time, and the lotion was the same. System for 1 mL/min, collecting all the column solution in the blowing nitrogen tube, at 45 ℃ blowing nitrogen concentrated to near dry, with methanol volume to 1.0 mL, then Add 1.0 mL of deionized water, vortex oscillation uniform, over 0.2 μm organic filter, to be tested. 7.2.2 Honey The concentrated solution was passed through an ammonia column (500 mg) and 4 mL of ethyl acetate was eluted three times at a flow rate of 1 mL/min. Blowing nitrogen tube, at 45 ° C blowing nitrogen concentrated dry, with methanol volume to 1.0 mL, then add 1.0 mL of deionized water, vortex oscillation uniform 0.2 μm organic filter, to be tested. 7.3 Determination 7.3.1 Gel chromatographic purification conditions 7.3.1.1 Gel purification column. Bio-Beads, S-X3, 300 mm × 25 (inner diameter) mm; 38 μm to 75 μm. 7.3.1.2 Concentration temperature. 45 ° C. 7.3.1.3 Mobile phase. cyclohexane-ethyl acetate (50 50, volume ratio). 7.3.1.4 constant volume reagent. acetonitrile. 7.3.1.5 Flow rate. 4.7 mL/min. 7.3.1.6 Injection volume. 5 mL. 7.3.2 LC-MS/MS mass spectrometry reference conditions 7.3.2.1 Reference conditions for liquid chromatography A) Column. Waters Atlantis Hilic Silica column, 3 μm, 3.0 mm (id) x 50 mm, or equivalent. B) Column temperature. 40 ° C. C) mobile phase. methanol - water (90 10, volume ratio). D) Flow rate. 0.30 mL/min. E) Injection volume. 10 μL. 7.3.2.2 Reference conditions for mass spectrometry determination See Appendix A. 7.3.3 Determination and confirmation of chromatography According to the content of thiamizole in the sample solution, the standard working solution with similar peak area is selected. Standard working solution and sample solution of thiamylamine The response value shall be within the linear range of the instrument detection. Standard working solution and sample solution volume measurement. Under the above chromatographic conditions, thiophene The retention time of the amylamine is about 1.01 min. The selected component selects one parent ion and two or more daughter ions. Under the same experimental conditions, The sample in the sample to be tested and the standard solution corresponding to the retention time deviation within ± 2.5%; and the sample spectrum of each component of the qualitative ions Relative abundance and concentration of the standard solution in the standard solution corresponding to the relative abundance of qualitative ions were compared, the deviation does not exceed the provisions of Table 1 The samples were confirmed to be positive for thiamylamine detection. The spectrum of the standard is shown in Appendix B, Figures B.1, B.2. Table 1 Maximum allowable deviation of relative ion abundance when qualitative confirmation 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 the following formula (1) to calculate the content of thiadiazole pesticide in the sample, the calculation result is deducted from the blank value. Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10% Allowable relative deviation ± 20% ± 25% ± 30% ± 50% MA VcA S    .. (1) Where. The residual content of thiamylamine in X - sample solution is in ng/g (ng/g); The peak area of thiazolylamine in A - sample solution; C - the concentration of thiamylamine in the standard working solution in ng/ml (ng/mL); V - Final volume of the final solution in milliliters (mL); AS - standard chromatographic peak area of thiamylamine in standard working solution; M - the final sample on behalf of the sample quality, in grams (g). Note. The result of the calculation should be deducted from the blank value. The result of the measurement is expressed by the arithmetic mean of the parallel measurement, and the two valid digits are retained.

9 precision

9.1 The ratio of the absolute difference between the two independent determinations obtained under reproducible conditions and their arithmetic mean (percentage) shall be in accordance with the Record the requirements of D. 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 the Record the requirements of E. 10% limit and recovery rate 10.1 Quantitation limits The limit of quantification of the method is less than 10 μg/kg. 10.2 Recovery rate When adding levels of 10 μg/kg, 20 μg/kg, 50 μg/kg, the addition rates of thiazolylamine in different matrices are given in Appendix C.

Appendix A

(Informative) Reference to mass spectrometry conditions Reference to mass spectrometry conditions A) ion source. electrospray ion source (ESI). B) Scan mode. negative ion scanning. C) Detection method. Multi-reaction selective ion detection (MRM). D) Electrospray voltage (IS). 4500V. E) atomization gas, air curtain gas, auxiliary heating gas, collision gas are high purity nitrogen and other suitable gas; before use should adjust the gas flow So that the mass spectrometry sensitivity reaches the detection requirement. F) Auxiliary gas temperature (TEM). 500 ° C. G) ion source temperature. 500 ° C. H) Qualitative ion pairs, quantitative ion pairs, acquisition time, deblocking voltage and collision energy are shown in Table A.1. Table A.1 thiamidonamine monitoring of ion pairs, quantitative ion pairs, deblocking voltage and collision energy Name of the test object Monitor ion pairs / (M/z) Quantitative ion pair / (M/z) Dwell time / (Ms) To cluster voltage / (V) Collision energy / (V) Thiamidomide 265.9/70.9 265.9/70.9 100 -61 -35 265.9/237.9 -15 Note. For different mass spectrometry instruments, the instrument parameters may be different, before the determination of the mass spectrometry parameters should be optimized to the best. Non-commercial declaration. The reference mass spectrometry conditions listed in Appendix A are done on the API3000 LC/MS, where the test instrument model is provided for Test, does not involve commercial purposes, to encourage standard users to try different manufacturers or models of equipment.

Appendix B

(Informative) Liquid samples of LC/MS-MS Figure B.1 Thiadiazole standard standard ion full-scan mass spectrometry Figure B.2 Thiamidamine Standard Multi-Reaction Monitoring (MRM) Chromatogram (10 μg/L)

Appendix C

(Informative) Table C, 1 The recovery rate of thiamidomide pesticides in different matrices Sample Substrate Add Concentration (μg/kg) Recovery (%) grape 10 92.4 ~ 108.0 20 78.5 ~ 95.0 50 71.8 ~ 91.0 lettuce 10 78.6 ~ 91.6 20 88.5 to 105.0 50 76.0 ~ 95.8 Cabbage 10 100.0 ~ 109.0 20 89.5 to 108.0 50 97.8 ~ 107.8 Tangerine 10 99.4 ~ 109.0 20 89.0 ~ 107.5 50 98.6 ~ 110.2 Chestnut 10 87.7 ~ 110.0 20 76.0 ~ 104.5 50 90.6 ~ 105.8 carrot 10 93.4 ~ 110.0 20 91.0 ~ 117.0 50 87.4 ~ 109.4 ketchup 10 92.0 to 102.0 20 88.0 to 104.5 50 90.8 ~ 101.6 chicken 10 90.7 to 103.0 20 87.5 ~ 104.5 50 87.6 ~ 97.4 Tilapia 10 88.4 to 104.0 20 90.0 to 99.0 50 86.6 ~ 94.4 400 82.0 ~ 105.8 beef 10 67.7 ~ 87.4 20 86.5 ~ 100.0 50 96.8 ~ 105.6 Sheep liver 10 72.8 ~ 95.7 20 78.5 ~ 109.5 50 68.2 to 101.4 Rice 10 90.7 to 109.0 50 90.0 to 104.0 100 93.2 ~ 104.4 1000 103.8 ~ 111.0 tea 10 77.4 ~ 93.4 20 83.0 ~ 116.0 50 79.6 ~ 99.2 honey 10 85.0 to 105.0 20 75.5 to 104.5 50 79.8 ~ 87.2

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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