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GB 23200.30-2016 English PDF

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GB 23200.30-2016: Food safety national standard -- Determination of cyclophosphamide residues in foodstuffs by gas chromatography-mass spectrometry
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Standard similar to GB 23200.30-2016

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Basic data

Standard ID GB 23200.30-2016 (GB23200.30-2016)
Description (Translated English) Food safety national standard -- Determination of cyclophosphamide residues in foodstuffs by gas chromatography-mass spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 11,155
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 1981-2007
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 23200.30-2016: Food safety national standard -- Determination of cyclophosphamide residues in foodstuffs by gas chromatography-mass spectrometry


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Food safety national standard - Determination of cyclophosphamide residues in foodstuffs by gas chromatography - mass spectrometry National Standards of People's Republic of China GB Instead of SN/T 1981-2007 National standards for food safety Determination of cyclophosphamide residues in food Gas chromatography - mass spectrometry National food safety standards- Determination of cyflufenamid 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

Foreword

This standard replaces SN/T 1981-2007 "Determination of cyclophosphamide residue in export food by gas chromatography-mass spectrometry". The main changes in this standard compared with SN/T 1981-2007 are as follows. - Standard text format is modified to national standard text format for food safety; - the name and scope of the "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 1981-2007. National standards for food safety Determination of cyclophosphamide residues in foodstuffs by gas chromatography - mass spectrometry

1 Scope

This standard specifies the preparation of cyclophosphamide residues in food and gas chromatography-mass spectrometry. This standard applies to wheat, corn, peanuts, pineapples, apples, green onions, carrots, basil leaves, honeysuckle, ginger powder, pepper powder and Determination and confirmation of cyclophosphamide residues in tea, and other foods may be referred 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 the extract, and the solution was dehydrated with sodium chloride. The samples were washed with Envi-Carb/LC-NH2 column or C18 solid phase extraction column or Florisil Column chromatography, gas chromatography - 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 Acetonitrile (C2H3N). Chromatographic pure. 4.1.2 n-hexane (C6H14). pure chromatography. 4.1.3 Acetone (C3H6O). Chromatographic pure. 4.1.4 ether (C4H10O). chromatographic purity. 4.1.5 Toluene (C7H8). Chromatographic pure. 4.1.6 sodium chloride (NaCl). excellent grade pure. 4.1.7 anhydrous sodium sulfate (Na2SO4). analytical pure, 650 ℃ burning 4 h, after natural cooling stored in a sealed bottle in reserve. 4.2 solution preparation 4.2.1 Phosphate buffer. 0.5 mol/L (pH = 7.0), weigh 52.7 g of dipotassium hydrogen phosphate (K2HPO4) and 30.2 g of potassium dihydrogen phosphate (KH2PO4), add about 500 mL of water dissolved, with 1 mol/L sodium hydroxide or 1 mol/L hydrochloric acid to adjust pH7.0, add water to volume 1L. 4.3 standards 4.3.1 Reference substance. Cyflufenamid, C22H17F5N2O2, CASNO. 180409-60-3, purity ≥98%; 4.4 standard solution preparation 4.4.1 cyclofluramine standard stock solution. Weigh the appropriate amount of cyclofluoride standard, with acetone - n-hexane (1 1) prepared into 1.0 mg/mL standard Quasi-stock solution; 0-4 0C save. 4.4.2 Cyclofluorescein Standard working solution. Prepare the stock solution with acetone-n-hexane (1 1, V/V) as required. Quasi working fluid. 0-4 0C save. 4.5 Materials 4.5.1 Envi-Carb/LC-NH2 solid phase extraction column. 500 mg/500 mg. 4.5.2 C18 solid phase extraction column. 1000 mg. 4.5.3 Florisil. Florisil, 0.150-0.250 mm; 4.5.4 Florisil Column. The glass column 30 cm × 15 mm (id) was charged with 1 cm high anhydrous sodium sulfate, 10 g Florisil and 1 cm high anhydrous sodium sulfate.

5 instruments and equipment

5.1 Gas Chromatography-Mass Spectrometer. Equipped with an electronically bombarded ion source (EI source). 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 Oscillator. 5.4 whirlpool mixer. 5.5 Rotary Evaporator. 5.6 high speed homogenizer. 5.7 Centrifuge. 5.8 Centrifuge tube. 100 mL. 5.9 Separate funnel. 150 mL. 5.10 Filtration. 0.45 μm.

6 Preparation and storage of samples

6.1 Preparation of the sample 6.1.1 wheat, rice, 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 fruit or vegetables 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 ℃; fruit and vegetable samples at -18 ℃ below the cold Frozen save. 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 Grains, nuts Weigh 10 g of sample (accurate to 0.01 g) in a 100 mL centrifuge tube and add 20 mL of water for 5 min. Plus 50 mL of acetonitrile at 10,000 R/min homogeneous extraction 1 min, centrifugation 3 min, the extract into the 100 mL volumetric flask. The residue was then repeated with 2 x 20 mL of acetonitrile Extract twice. The extracts were combined and bound to 100 mL with acetonitrile. Accurately absorb 20 mL of the extract in a 150 mL separatory funnel, followed by addition 10 g of sodium chloride and 20 mL of phosphate buffer, shaken for 3 min. After standing, discard the water layer. 7.1.2 fruits, vegetables Weigh 20 g sample (accurate to 0.01 g) in 100 mL centrifuge tube, add 50 mL of acetonitrile, homogenize at 10,000 r/min for 1 min, centrifuge 3 min, the extract into the 100 mL volumetric flask, the residue and then were 2 × 20 mL acetonitrile repeated extraction twice, the combined extract, Acetonitrile to 100 mL. Accurately absorb 20 mL of the extract in a 150 mL separatory funnel, add 10 g of sodium chloride and 20 mL of phosphate buffer Liquid, shaking 3 min. After standing stratification, discard the water layer. Acetonitrile layer by adding 5 g of anhydrous sodium sulfate dehydration at 45 ° C rotation concentrated to near dry, Add 2 mL of acetonitrile-toluene (3 1) mixed solution to dissolve. 7.1.3 seasonings, Chinese herbal medicine Weigh 5 g of sample (accurate to 0.01 g) in a 100 mL centrifuge tube and add 10 mL of water for 15 min. Plus 50 mL of acetonitrile at 10,000 R/min homogeneous 1 min, centrifugation 3 min, the extract into the 100 mL volume of the product, the residue and then 2 × 20 mL acetonitrile repeated extraction twice, The extracts were combined and bound to 100 mL with acetonitrile. Accurately remove 20 mL of the extract in a 150 mL separatory funnel and add 10 g of sodium chloride in turn And 20 mL of phosphate buffer, shaking 3 min. Static separation, abandoned the lower water. The acetonitrile layer was added with 5 g of anhydrous sodium sulfate and dehydrated at 45 ° C Concentrated to near dry, with n-hexane volume to 5 mL. 7.1.4 Tea Weigh the sample 1 g (accurate to 0.01 g) in a 50 mL centrifuge tube, add 1 g of sodium chloride and 3 mL of water on a vortex mixer Fully mixed for 1 min, placed 0.5 h, adding 10 mL of n-hexane - acetone (1 1) mixed solution to 10000 r/min homogenization 1 min, Centrifuged 3 min, the upper organic phase was taken over anhydrous sodium sulfate in a concentrated flask and the residue was washed with 2 x 20 mL of n-hexane-acetone (1 1) The extraction was repeated twice, and the combined organic phases were combined and concentrated in a 45 ° C water bath under reduced pressure to near dryness. 7.2 Purification 7.2.1 Grains, nuts C18 column was pre-eluted with 10 mL of acetonitrile and the effluent was discarded. The acetonitrile extract was injected and eluted with 2 mL of acetonitrile to collect the whole eluent, Dehydrated by anhydrous sodium sulfate, concentrated to near dry at 45 ° C, and dissolved with 2 mL of acetonitrile-toluene (3 1) mixed solution. The Envi-carb/LC-NH2 (500 mg/500 mg) column was pre-leached with 10 mL of acetonitrile-toluene (3 1) mixed solution to discard the effluent. The resulting solution was poured and rinsed with 25 mL of a mixed solution of acetonitrile-toluene (3 1). The eluate was collected and concentrated at 45 ° C to near- The residue was dissolved in 1.0 mL acetone-n-hexane (1 1) mixed solution and passed through a 0.45 μm filter and analyzed by gas chromatography-mass spectrometry. 7.2.2 vegetables, fruits Envi-carb/LC-NH2 (500 mg/500 mg) was eluted with 10 mL of acetonitrile-toluene (3 1) mixed solution and the effluent was discarded. The resulting extract was injected into 7.1.2 and eluted with 25 mL of acetonitrile-toluene (3 1) mixed solution. The eluate was collected and concentrated to near dryness at 45 ° C. The residue was dissolved in 1.0 mL acetone-n-hexane (1 1) mixed solution and passed through a 0.45 μm filter and analyzed by gas chromatography-mass spectrometry. 7.2.3 seasonings, Chinese herbal medicine The florisil silica column was eluted with 30 mL of n-hexane and the effluent was discarded. Add 2 mL of 7.1.3 of the extract to the column with 100 mL N-hexane-diethyl ether (17 3), and the eluate was collected and concentrated to near dryness at 45 ° C. The residue was washed with 1 mL of acetone n-hexane (1 1) Mixed solution solution, over 0.45 μm filter, gas chromatography - mass spectrometry. 7.2.4 Tea The residue was dissolved in 5 mL of n-hexane and transferred to a Florisil column. Rinse with 5 mL n-hexane, discard the effluent, with 5 mL positive Hexane-ether (9 1) mixed solution. The eluate was collected in a 10 mL centrifuge tube and slowly blown in a 45 ° C water bath with a nitrogen bubbler The residue was dissolved in 1 mL of acetone-n-hexane (1 1) mixture and passed through a 0.45 μm filter and analyzed by gas chromatography-mass spectrometry. 7.3 Determination 7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions A. Column. DB-35MS quartz capillary column. 30 m × 0.25 mm (id), 0.25 μm (film thickness) B. Column temperature. 70 ° C 25 ° C/min 260 ° C (1 min) 5 ° C/min 300 ° C (10 min) C. Inlet temperature. 250 ° C D. Auxiliary heater. 280 ° C; E. Ion source temperature. 230 ° C; F. Quadrupole temperature. 150 ° C G. Carrier gas. helium purity ≥99.999%, 1 mL/min; H Injection volume. 2 μL I injection mode. pulse does not split J. Ionization mode. EI K Ionization energy. 70eV L. Select ions. (m/z) 412,321,294,275, Quantitative ions 412 7.3.2 Determination and confirmation of chromatography According to the sample solution content of the sample, the selected concentration of similar standard working solution, the standard working solution and sample volume and other volume insert The response value of cyclofluramine in the standard working solution and the sample to be measured shall be within the linear range of the instrument detection. If the sample solution is in the selective ion chromatogram of the standard working solution, a chromatographic peak appears at the same retention time, and after subtracting the background After the sample quality chromatogram, the selected ions are present, the abundance of the selected ions is proportional to the abundance ratio of the corresponding ions of the standard. Within the allowable range (see Table 1). Under the condition of 6.3.1, the retention time of cyclofluramine was 10.0 min, and the monitoring ion (m/z) Which was confirmed by m/z 412,321,294,275 (the abundance ratio was 100. 70. 85. 50); according to the quantitative ion m/z421 Line outside the standard method. Under the conditions of 6.3.1, the total ion chromatogram and full scan mass spectrum of the cyclofluramine standard were analyzed by gas chromatography-mass spectrometry Appendix A, Figure A.1 and Appendix B, Figure B.1. Table 1 Maximum qualitative error of relative ion abundance when qualitative gas chromatography-mass spectrometry Relative ion abundance > 50% > 20% to 50% > 10% to 20% ≤10% Maximum permissible 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

The amount of cyclofluramine residues in the sample was calculated using a chromatographic data processor or by equation (1). A × c × V AS x m (1) Where. X - the amount of cyclophosphamide residues in milligrams per kilogram (mg/kg); A - peak area of cyclofluramine in sample solution; AS - peak area of standard working solution of cyclofluramine; V - the final volume of the sample solution in milliliters (mL); The concentration of C - cyclofluoromide standard working solution is in micrograms per milliliter (μg/mL); 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 C 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 D requirements. 10% limit and recovery rate 10.1 Quantitation limits The limits of the method of cyclofluramine. wheat, corn, peanuts, pineapple, apple, green onions, carrots 0.005 mg/kg. Basil Leaves, honeysuckle, ginger powder, pepper powder and tea in the 0.010 mg/kg. 10.2 Recovery rate The experimental data on the concentration and recovery of the sample are given in Appendix B. X =

Appendix A

(Informative) Selective ion flow chart of cyclophosphamide standard substance Figure A1 cyclofluramine standard selection ion flow diagram Figure A2 Selective ion spectrum of cyclofluoride standard

Appendix B

(Informative) Sample concentration and recovery of the experimental data Table B.1 Experimental data on the concentration and recovery of the sample sample name Add concentration (Μg/kg) Recovery rate(%) Pepper 10 84.75 ~ 106.45 20 82.10 ~ 107.78 40 89.06 ~ 101.72 Ginger powder 10 84.65 ~ 100.90 20 82.08 ~ 110.55 40 83.10 ~ 103.51 Hu Lo Bu 5.0 90.80 to 107.80 10 90.33 ~ 95.90 20 94.06 ~ 108.44 Green onions 5.0 90.10 to 95.40 10 83.20 to 99.90 20 91.94 ~ 99.55 apple 5.0 92.30 to 101.30 10 91.43 ~ 116.93 20 92.08 to 108.51 Pineapple 5.0 97.00 ~ 104.50 10 94.53 ~ 103.23 20 90.01 ~ 109.50 corn 5.0 80.90 ~ 92.70 10 86.65 ~ 101.30 20 79.80 ~ 95.78 wheat 5.0 81.20 ~ 111.40 10 85.25 ~ 92.05 20 83.48 ~ 96.53 peanut 5.0 75.00 ~ 100.70 10 90.80 to 109.00 20 86.13 to 118.15 tea 10 83.30 ~ 107.00 20 77.60 ~ 104.80 40 81.50 to 102.00 honeysuckle 10 81.60 ~ 98.50 20 80.40 ~ 93.12 40 84.46 ~ 94.42 Basil 10 84.35 ~ 101.70 20 82.85 ~ 103.45 40 84.14 ~ 98.88

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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