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GB 23200.67-2016 English PDF

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GB 23200.67-2016: Food safety national standard -- Determination of residual alkynyl chloride residues in foodstuffs by gas chromatography-mass spectrometry
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Standard similar to GB 23200.67-2016

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Basic data

Standard ID GB 23200.67-2016 (GB23200.67-2016)
Description (Translated English) Food safety national standard -- Determination of residual alkynyl chloride residues in foodstuffs by gas chromatography-mass spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 11,181
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 2647-2010
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 23200.67-2016: Food safety national standard -- Determination of residual alkynyl chloride residues in foodstuffs by gas chromatography-mass spectrometry


---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Food safety national standards - Determination of residual alkynyl chloride residues in foodstuffs by gas chromatography - mass spectrometry Replace SN/T 2647-2010 National standards for food safety Determination of the Residue of Acetyl Acetate in Food Gas chromatography - mass spectrometry National food safety standards- Determination of propyzamide residue in foods Gas 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 GB National Standards of People's Republic of China

Foreword

This standard replaces SN/T 2647-2010 "Determination of the amount of acetylene acenamide residues in import and export food by gas chromatography-mass spectrometry". Compared with SN/T 2647-2010, 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 2647-2010. National standards for food safety Determination of residual alkynyl chloride residues in foodstuffs by gas chromatography - mass spectrometry

1 Scope

This standard specifies the method of gas chromatography-mass spectrometry for the separation of acetophenone residues in food. This standard applies to spinach, carrots, strawberries, peanuts, chicken, onions, cod, honey, chestnut and tea The detection and confirmation of residues, 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 date of the note applies This document. 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 sample was extracted with acetonitrile and purified by liquid-liquid partitioning and propyl ethylenediamine-bonded silica gel (PSA) solid phase extraction column. Determination of mass spectrometry by gas chromatography - electron bombardment and external standard method.

4 reagents and materials

Unless otherwise specified, the reagents used are of analytical grade and the water is in accordance with the primary water specified in GB/T 6682. 4.1 Reagents 4.1.1 Acetone (C3H6O). Pesticide Residue. 4.1.2 acetonitrile (C2H3N). pesticide residues. 4.1.3 N-Hexane (C6H14). Pesticide Residue. 4.1.4 sodium chloride (NaCl). 650 ℃ burning 4 h, placed in a dryer cooling, standby. 4.2 solution preparation 4.2.1 acetonitrile saturated n-hexane. take 100mL n-hexane, 100mL acetonitrile in the separatory funnel, the oscillation mix, take the upper stand. 4.2.2 n-hexane saturated acetonitrile. take 100mL n-hexane, 100mL acetonitrile in the separatory funnel, shake mix, take the next stand. 4.2.3 Acetone-n-Hexane (3 7, V/V). Take 300 mL of acetone and add 700 mL of n-hexane to shake. 4.3 standards 4.3.1 Acetylacetamide standard substance (propyzamide, molecular formula. C12H11Cl2NO, molecular weight 255, CAS 5.2 solid phase extraction device. 5.3 homogenizer, speed 10000 r/min. 5.4 Rotary Evaporator. 5.5 nitrogen concentrator. 5.6 with a plug centrifuge tube. 50 mL, 100 mL. 5.7 Concentrated bottles. 50 mL, 100 mL. 5.8 Analytical balance. 0.01 g and 0.0001 g.

6 Preparation and storage of samples

6.1 Preparation of the sample 6.1.1 Grains and nuts Take a representative sample volume of 500g, all ground and pass through a 2.0 mm round hole screen. Mix well, into a clean container, sealed, Mark the mark. 6.1.2 Fruits and vegetables Take a representative sample 500g, chopped (not washable), with a food mashed machine to sample into a slurry. Mix well and put it clean Of the container, sealed, marked mark. 6.1.3 Meat and fish Take a representative sample 500g, fully crushed evenly, into a clean container as a sample. Sealed, marked. 6.1.4 honey Take a representative sample 500g, the crystallization of honey samples will be evenly stirred; on the crystallization of honey samples, in the closed The case, the sample bottle placed in not more than 60 ℃ in the water bath in the warm, shaking, until the sample all melted and stir well, quickly cooled to room temperature, In the melting must pay attention to prevent moisture evaporation. Load a clean container, sealed, marked with a mark. 6.1.5 Tea Take a representative sample of 500 g, grind all with an attritor and pass through a 2.0 mm round hole screen. Mix well and clean the clean container Inside, sealed, marked mark. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 6.2 Sample storage Grains and nuts are stored at 0 to 4 ° C; other samples are cryopreserved at -18 ° C or lower. During the operation of the sample preparation, the sample should be protected from contamination or changes in the content of the residue.

7 Analysis steps

7.1 Extraction Weigh 10 g of sample (accurate to 0.01 g) in a 100 mL stoppered centrifuge tube, add 10 mL of water, add 40.0 mL Hexane saturated acetonitrile, homogenizer extraction 2 min (honey plus water 10mL and acetonitrile to be vigorous oscillation 20min), then add 5g sodium chloride, Severe oscillation 10min, 3000 r/min centrifugal 10min, to be purified. 7.2 Purification 7.2.1 Liquid/liquid distribution purification Take the upper extract 20.0 mL (spinach, carrot, strawberry) or 10.0 mL (peanuts, chicken, onions, cod, honey, chestnut And tea) were transferred to a 50 mL stoppered centrifuge tube, 10 mL of acetonitrile was added to the saturated n-hexane, shaken for 3 min, left to stand, discarded The n-hexane phase was removed and the n-hexane phase was discarded again with 10 mL of acetonitrile saturated n-hexane. The lower acetonitrile phase was collected in 100 mL Concentrated in a 40 ° C water bath and concentrated to approximately 1 mL. 7.2.2 Solid phase extraction (SPE) purification The PSA column was pre-leached with 5 mL of acetone-n-hexane. The sample solution was poured into the column and eluted with 10 mL of acetone-n-hexane to control the flow rate At 2 mL/min. The whole eluate was collected and concentrated to near dryness in a water bath at 40 ° C. Dissolved with acetone - n - hexane and set to 1.0 mL, determined by gas chromatography-mass spectrometry. 7.3 Determination 7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions A) Column. HP-5 MS quartz capillary column, 30 m × 0.25 mm (id), film thickness 0.25 μm, or equivalent; B) column temperature. the initial temperature of 70 ℃, keep 2 min, 25 ℃/min program temperature to 150 ℃, 3 ℃/min procedures Heated to.200 ℃, and then 8 ℃/min program to 280 ℃, keep 10 min; C) Inlet temperature. 250 ° C; D) chromatographic - mass spectrometer interface temperature. 280 ° C; E) Carrier gas. helium, purity greater than or equal to 99.999%, constant pressure mode, 144kpa; F) Injection volume. 1 μL; G) Injection method. no split injection, 0.65 min after the opening valve; H) ionization mode. electron bombardment; I) ion source temperature. 230 ° C; J) quadrupole temperature. 150 ° C; L) Determination of the way. select the ion monitoring mode; M) Select the monitoring ion (m/z). Quantitative 173, Qualitative 175,145,255; N) solvent delay. 4.0 min. 7.3.2 Determination and confirmation of chromatography According to the content of the sample in the sample, select the concentration of similar matrix standard working solution, the standard working solution and sample solution The response values of the solution in the matrix standard working solution and the sample solution are determined in the linear range of the instrument Inside. If the sample solution is in the selective ion chromatogram of the standard working solution, a chromatographic peak appears at the same retention time, In the sample quality chromatogram, the selected ions are present, the abundance of the selected ions is greater than the abundance ratio of the corresponding ions Within the allowable range (see Table 1). Under the above chromatographic conditions, the acetophenolide retention time was about 14.0 min, which monitored the ions (M/z) m/z 173, 175, 145, 255 (the relative abundance ratio of 100. 72. 24. 36) to confirm it; according to quantitative ions M/z173 for its external standard method. Chromatography-mass spectrometry total ion chromatogram of the acetophenone chloride standard under the above chromatographic conditions And full scan mass spectra are shown in Appendix A, Figures A.1 and A.2. Table 1 Confirmation of relative ion abundance maximum allowable error Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10% Allowable relative deviation ± 20% ± 25% ± 30% ± 50% 7.4 blank test In addition to the sample, according to the above steps.

8 results are calculated and expressed

Use the chromatographic data processor or (1) to calculate the amount of acetophenamide residues in the sample. H × c × V X = - - - - (1) Hs × m Where. X - the amount of acetophenamide residues in milligrams per kilogram (mg/kg); H - sample solution of acetophenone chloride peak high; C - the concentration of acetophenamide in standard working solution, in micrograms per milliliter (μg/mL); V - the final volume of the sample solution in milliliters (mL); Hs - the standard working solution of acetophenone chloride peak high; M - the mass of the sample represented by the final sample, in grams (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) Together with the requirements of Appendix C. 9.2 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) Together with the requirements of Appendix D. 10% limit and recovery rate 10.1 Quantitation limits The limit of quantification of the method is 0.01 mg/kg. 10.2 Recovery rate When the levels were 0.01 mg/kg, 0.02 mg/kg, 0.04 mg/kg, the addition of acetophenone was given in Appendix B.

Appendix A

(Informative) Total Ion Chromatogram and Mass Spectrometry of Reference Material of 8 .0 0 9 .0 0 1 0. 0 0 1 1 .0 0 1 2 .0 0 1 3. 0 0 1 4 .0 0 1 5 .0 0 1 6 .0 0 1 7 .0 0 1 8 .0 0 1 9 .0 0 1 e 0 7 1 .2 e 0 7 1 .4 e 0 7 1 .6 e 0 7 1 .8 e 0 7 2 e 0 7 2 .2 e 0 7 2 .4 e 0 7 Time - - > Abundance TIC. SCAN .D \\ data .ms 9 .3 9 4 1 4 .0 8 6 Figure A.1. Total ion chromatogram of the standard material of the acetophenamide 5 0 1 0 0 1 5 0 2 0 0 2 5 0 3 0 0 3 5 0 4 0 0 4 5 0 5 0 0 M/z - - > Abundance Scan 1 1 9 2 (1 4 .0 6 8 points). SCAN .D \\ data .ms 1 7 3 .0 2 5 5 .0 1 0 9 .0 7 4 .1 2 1 2 .0 3 3 1 .0 4 2 9 .72 9 3 .2 3 7 5 .2 5 0 5 .5 Figure A.2 Spectrum of the standard material of acetophenamide

Appendix B

(Informative) The recovery rate was added to different matrices Table B.1 Recovery rates in different substrates Sample concentration (mg/kg) Recovery rate range (%) Sample addition concentration (mg/kg) Recovery rate range (%) spinach 0.01 80.0 to 110.0 Codfish 0.01 92.0 to 110.0 0.02 87.5 to 112.5 0.02 91.5 to 104.5 0.04 95.0 to 115.0 0.04 93.0 to 112.0 carrot 0.01 94.0 to 111.0 honey 0.01 92.0 to 110.0 0.02 90.0 to 107.0 0.02 92.6 to 102.5 0.04 96.0 to 105.0 0.04 95.5 to 105.0 Strawberry 0.01 91.0 to 110.0 Chestnut 0.01 85.0 to 110.0 0.02 97.0 to 105.5 0.02 92.5 to 117.5 0.04 97.0 to 105.0 0.04 95.0 to 106.0 peanut 0.01 90.0 to 110.0 tea 0.01 92.0 to 110.0 0.02 97.5 to 107.5 0.02 97.5 to 112.5 0.04 98.0 to 107.0 0.04 98.05 to 103.0 chicken 0.01 95.0 to 110.0 0.01 95.0 to 110.0 0.02 94.0 to 107.5 0.02 97.5 to 115.0 0.04 95.0 to 106.0 0.04 95.0 to 110.0

Appendix C

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

Appendix D

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

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