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GB 23200.64-2016 English PDF

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GB 23200.64-2016: Food safety national standard -- Determination of Residual Potassium Acetate in Food by Liquid Chromatography -- Mass Spectrometry / Mass Spectrometry
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GB 23200.64-2016English219 Add to Cart 3 days [Need to translate] Food safety national standard -- Determination of Residual Potassium Acetate in Food by Liquid Chromatography -- Mass Spectrometry / Mass Spectrometry Valid GB 23200.64-2016

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Standard similar to GB 23200.64-2016

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Basic data

Standard ID GB 23200.64-2016 (GB23200.64-2016)
Description (Translated English) Food safety national standard -- Determination of Residual Potassium Acetate in Food by Liquid Chromatography -- Mass Spectrometry / Mass Spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 11,150
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 2623-2010
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 23200.64-2016: Food safety national standard -- Determination of Residual Potassium Acetate in Food by Liquid Chromatography -- Mass Spectrometry / Mass Spectrometry


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Food safety national standard - Determination of Residual Potassium Acetate in Food by Liquid Chromatography - Mass Spectrometry/Mass Spectrometry National Standards of People's Republic of China GB Instead of SN/T 2623-2010 National standards for food safety Determination of Residual Potassium Propylate in Food Liquid chromatography - mass spectrometry/mass spectrometry National food safety standards- Determination of pyriproxyfen 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 2623-2010 "Liquid Chromatography-Mass Spectrometry/Mass Spectrometry" for the determination of pyruvate residues in food for import and export. Compared with SN/T 2623-2010, 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/T 2623-2010. National standards for food safety Determination of Residual Potassium Acetate in Food by Liquid Chromatography - Mass Spectrometry/Mass Spectrometry

1 Scope

This standard specifies the preparation and determination of the content of pyruvate residues in food. This standard applies to rice, soybeans, spinach, lemon, tea, mushrooms, beef, liver and milk in the detection of dibutyl ether 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 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 residual pyridyl ether in the sample was extracted with acidic acetonitrile under the action of sodium acetate buffer and purified by PSA packing. The liquid chromatography-mass spectrometry Determination of the 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 anhydrous magnesium sulfate (MgSO4). 4.1.2 anhydrous sodium acetate (C2H3O2Na). 4.1.3 acetic acid (C2H4O2). chromatography grade. 4.1.4 Acetonitrile (C2H3N). Chromatographic grade. 4.1.5 N-propyl ethylenediamine (PSA) filler. 50 m, chromatographic grade. 4.1.6 Formic acid (CH2O2). Chromatographic grade. 4.1.7 Ammonium acetate (C2H7NO2). 4.2 solution preparation 4.2.1 0.025% formic acid aqueous solution (containing 5 mmol/L ammonium acetate). accurately absorb 0.25 mL formic acid and weigh 0.386 g ammonium acetate in 1 L volumetric flask, dissolved in water and diluted to 1 L. 4.2.2 1% acetic acid in acetonitrile solution. 4.3 standards 4.3.1 Pyridine ether standard (Pyriproxyfen, C20H19NO3, CAS. 95737-68-1). purity > 99%. 4.4 standard solution preparation 4.4.1 Pyridyl ether standard stock solution. accurately weighed the appropriate amount of pyridyl ether standard, dissolved in acetonitrile and diluted with 100 μg/mL standard Quasi-stock solution, stored below 4 ℃. 4.4.2 Pyridyl ether standard working solution. If necessary, with 10% acetonitrile aqueous solution diluted to the appropriate concentration of standard working fluid, 4 ℃ below Save 4.5 Materials 4.5.1 Microporous membrane. 0.2 m, organic phase type.

5 instruments and equipment

5.1 Liquid Chromatography-Mass Spectrometry/Mass Spectrometer. Electrospray (ESI) ion source. 5.2 Centrifuge. 4 000 r/min. 5.3 Analysis of balance. 0.0001 g and 0.01 g. 5.4 plugs with polypropylene centrifugal tubes. 2 mL and 50 mL. 5.5 Crusher.

6 Preparation and storage of samples

6.1 rice, soybeans, spinach, lemon, tea, mushrooms, beef, liver Take a representative sample of about 500 g, with the tissue crusher fully mashed and mix, are divided into two, respectively, into the clean container as a test kind. Sealed and marked with mark. The sample was stored at -18 ° C and protected from light. 6.2 milk Take a representative sample of about 500 g, fully mixed, are divided into two, respectively, into a clean container as a sample, sealed, and marked mark. Store the sample below 4 ° C and store it in dark. During the operation of the sample preparation, the sample should be protected from contamination or changes in the content of the residue. Note. The above sample sampling site according to GB 2763 Appendix A implementation.

7 Analysis steps

7.1 Extraction 7.1.1 Tea, soybeans, mushrooms, rice samples Weigh the sample 5 g (accurate to 0.01 g) in a 50 mL polypropylene plastic centrifuge tube, add 10 mL of water, mix and let stand for 30 min. The centrifuge tube was placed in an ice bath and then 6 g of anhydrous magnesium sulfate and 1.5 g of anhydrous sodium acetate were added. After returning to room temperature, 15.0 mL 1% acetic acid in acetonitrile solution, shake extraction 4 min, 4000 r/min centrifugation 5 min. 7.1.2 Spinach, lemon and milk samples Weigh 15 g (accurate to 0.01 g) in 50 mL of polypropylene plastic pre-called 6 g of anhydrous magnesium sulfate and 1.5 g of anhydrous sodium acetate Centrifuge tube, the centrifuge tube placed in an ice bath, returned to room temperature, the accurate addition of 15.0 mL 1% acetic acid acetonitrile solution, the oscillation extraction 4 min, 4000 r/min centrifugation 5 min. 7.1.3 beef, liver samples Weigh 15 g (accurate to 0.01 g) in 50 mL polypropylene plastic centrifuge tube, accurately add 15 mL 1% acetic acid acetonitrile solution, shaking Extraction 4 min, 4000 r/min centrifugation 5 min. Also called 50 g of polypropylene plastic with 6 g of anhydrous magnesium sulfate and 1.5 g of anhydrous sodium acetate Centrifuge tube, add 10 mL of water, dissolved until the aqueous solution to room temperature, then the acetonitrile extract transferred to them, oscillation 4 min, 4000 R/min centrifugation 5 min. 7.2 Purification Take 1 mL of the above acetonitrile extract in a 2 mL polypropylene plastic centrifuge tube pre-called 50 mg PSA and 150 mg anhydrous magnesium sulfate, Oscillation was extracted for 1 min and centrifuged at 4000 r/min for 5 min. Accurately absorb.200 μL supernatant with water to 1 mL, mix well after 0.2 μm filter. The filtrate was subjected to liquid chromatography-mass spectrometry. 7.3 Determination 7.3.1 High Performance Liquid Chromatography Reference Conditions A) Column. Column. CAPCELL PAK C18 column, 50 mm x 2.0 mm (id), 3 μm or equivalent. B) Mobile phase. A. 0.1% formic acid acetonitrile solution, B. 0.025% formic acid aqueous solution (containing 5 mmol/L ammonium acetate). C) Flow rate. 300 μL/min, gradient elution program in Table 1. Table 1 gradient elution program table D) Column temperature. 35 ° C. E) Injection volume. 20 μL. 7.3.2 Mass spectrometry reference conditions A) ion source. electrospray ESI, positive ion. Gradient time/min mobile phase A /% mobile phase B /% / 4.5 20 80 8.5 20 80 B) Scanning mode. Multiple reaction monitoring (MRM). C) See Appendix A for other parameter conditions. 7.3.3 Quantitative determination According to the content of the sample in the sample, select the standard response of similar standard working fluid at the same time for analysis. Standard working solution and the test solution The reaction value of the propyl ether should be within the linear response range of the instrument. The reference retention time of pyridine ether under the above chromatographic conditions was 1.4 min The multi-reaction monitoring chromatogram of the quasi-solution is shown in Appendix B. 7.3.4 Qualitative determination Determination of sample and standard working solution according to liquid chromatography-mass spectrometry/mass spectrometry conditions if the mass retention time and standard The relative abundance of the qualitative ion pair is expressed as a percentage of the intensity relative to the strongest abundance, and should be comparable to the concentration As the relative abundance of the solution is consistent, the relative abundance tolerance does not exceed the range specified in Table 2, it can be judged that there is a corresponding measured Things. Table 2 The maximum allowable deviation of relative ion abundance when qualitative confirmation 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 calculate the amount of the drug to be tested in the sample according to formula (1). The result of the calculation is deducted from the blank value. A × c × V X = (1) As × m × 1000 Where. X - the content of pyridyl ether in the sample, in micrograms per kilogram (μg/kg); The peak area of pyridyl ether in A - sample solution; C - the concentration of pyridyl ether in the standard solution in micrograms per milliliter (μg/mL); V - the final volume of the sample solution in milliliters (mL); As - the peak area of pyridyl ether in standard solution; M - the mass of the sample represented by the final solution 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) 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 method of spinach, lemon, beef, liver and milk in the quantitative limit of 5.0 μg/kg; The limit of quantification in this method for soybean, rice, mushroom and tea is 15.0 μg/kg. 10.2 Recovery rate The recovery of the addition of pyridyl ether in different matrices is given in Appendix C.

Appendix A

(Informative) API 4000 Liquid Chromatography - Quad Column Tandem Mass Spectrometer Parameters 1) Monitor ion pairs and voltage, barometric parameters A) Ion source temperature. 350 C; B) electrospray voltage. 5250 V; C) Collision pressure. 34.475 kPa (5 psi); D) air curtain gas pressure. 206.85 kPa (30 psi) E) atomization gas pressure. 344.75 kPa (50 psi); F) Auxiliary gas pressure. 413.7 kPa (60 psi); G) pyrolysis ether quantitative ion pair, qualitative ion pair, deblocking voltage (DP), collision gas energy (CE) and retention time are shown in Table A.1. Table A.1 Pyridine Ether Quantitative Ion Pair, Qualitative Ion Pair, Discharge Voltage (DP), Collision Gas Energy (CE) and Retention Time Component name Qualitative ion pair m/z Quantitative ion pair m/z To cluster DP/v Collision energy CE/v keep time T/min Pyridine ether 322.2 → 185.0 322.2 → 185.0 110 1.4 322.2 → 227.2 14 1) Non-commercial notices. Appendix Table A.1 The parameters listed in the API 4000 mass spectrometer are listed here. The test instrument model is for reference only, Does not involve commercial purposes, encourage standard users to try different manufacturers and models of equipment

Appendix B

(Informative) Pyridyl Ether Multi - Reaction Monitoring (MRM) Chromatogram Figure B.1 Pyridyl ether MRM chromatogram

Appendix C

(Informative) Method to add concentration and recovery range Table C.1 Concentration of the concentration of pyridyl ether and recovery range Sample name Add concentration (μg/kg) Average recovery rate (%) Precision (%) Rice 15.0 89.3 ~ 107.3 9.2 100 83.5 ~ 101.3 6.4 200 86.3 ~ 102.1 6.9 spinach 5.0 81.4 ~ 101.8 7.2 50 86.2 ~ 103.8 7.0 100 79.7 ~ 101.3 8.8 lemon 5.0 70.6 ~ 100.4 10.9 50 73.8 ~ 103.2 6.2 500 80.1 ~ 100.2 8.5 tea 15.0 83.3 ~ 101.3 6.6 100 86.8 ~ 108.9 9.7 200 79.1 to 104.8 8.0 Liver 5.0 77.6 ~ 101.8 8.5 20 81.5 to 113.0 10.5 100 77.7 ~ 107.2 10.9 beef 5.0 80.6 ~ 99.8 7.5 10 83.5 to 106.0 8.3 100 80.5 ~ 108.2 10.9 milk 5.0 81.4 ~ 99.4 6.3 20 81.5 ~ 103.0 7.8 100 78.2 ~ 100.8 9.2 Soybeans 15 83.3 ~ 104.7 7.8 50 75.8 ~ 103.2 8.4 100 84.0 ~ 99.0 8.1 mushroom 15 84.7 ~ 104.0 7.1 100 83.1 to 106.8 8.1 600 82.9 ~ 103.1 8.8

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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