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GB 23200.101-2016 English PDF

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GB 23200.101-2016: Food safety national standard -- Determination of residues of acaricides in royal jelly by gas chromatography -- Mass spectrometry
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GB 23200.101-2016English239 Add to Cart 3 days [Need to translate] Food safety national standard -- Determination of residues of acaricides in royal jelly by gas chromatography -- Mass spectrometry Valid GB 23200.101-2016

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Standard similar to GB 23200.101-2016

GB/T 38211   GB/T 18418   GB/T 18419   GB 23200.109   GB 23200.110   GB 23200.108   

Basic data

Standard ID GB 23200.101-2016 (GB23200.101-2016)
Description (Translated English) Food safety national standard -- Determination of residues of acaricides in royal jelly by gas chromatography -- Mass spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 12,152
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 2571-2010
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 23200.101-2016: Food safety national standard -- Determination of residues of acaricides in royal jelly by gas chromatography -- Mass spectrometry


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Food safety national standard - Determination of residues of acaricides in royal jelly by gas chromatography - mass spectrometry National Standards of People's Republic of China GB Replace SN/T 2571-2010 National standards for food safety Determination of Residues of Acaricides in Royal Jelly Gas chromatography - mass spectrometry National food safety standards- Determination of multiple miticide residues in royal-jelly 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 2571-2010 "Import and export royal jelly in a variety of acaricide residues detection method of gas chromatography - mass spectrometry." Compared with SN/T 2571-2010, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - standard name "import and export royal jelly" to "royal jelly"; - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN/T 2571-2010. National standards for food safety Determination of residues of acaricides in royal jelly by gas chromatography - mass spectrometry

1 Scope

This standard provides the royal jelly in the mite ether, methyl grams of mites, acaricides, lei mites, ethyl keto mite, brom mite, dicofol, Determination and Confirmation of Residue of Pyridenopsis by Gas Chromatography - Mass Spectrometry. This standard applies to royal jelly in the acaricidal ether, methyl grams of mites, acaricides, lei acarics, ethyl methicillin, bromide mites, dicofol, Determination and confirmation of residues of pyridaben 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 residue of the acaricide in the sample was extracted with a mixed solvent of n-hexane acetone (1 1, v/v), purged with a Florisil column, and the gas phase Spectral - mass spectrometry - negative chemical source determination, 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 ether (C4H10O). pure chromatography. 4.1.2 n-hexane (C6H14). pure chromatography. 4.1.3 Acetone (C3H6O). Chromatographic pure. 4.1.4 Sodium chloride (NaCl). 4.1.5 anhydrous sodium sulfate (Na2SO4). 650 ℃ burning 4h, in the dryer to cool to room temperature, stored in a sealed bottle in reserve. 4.2 standards 4.2.1 acaricidal mite, methyl acaricides, acaricides, deer mites, ethyl methicillin, bromocarbide, dicofol, Purity ≥99%, see Appendix A. 4.3 standard solution preparation 4.3.1 acaricides, methyl methicillin, acaricides, lemi mite, ethyl methicillin, bromide mite, dicofol, Solution. Weigh the appropriate amount of standard material accurately, with n-hexane dubbed the concentration of 100 μl/mL standard stock solution. Store in 4 ℃ refrigerator. 4.3.2 acaricides, methicillin mites, acaricides, lei mites, ethyl methicillin, bromocarbide, dicofolidone, pyridaben standard work Liquid. Dilute the mixture with n-hexane to the appropriate concentration of the standard working solution. Store in 4 ℃ refrigerator. 4.4 Materials 4.4.1 Florisil Solid Phase Extraction Column. (1 g, 6 mL) or equivalent. Use a 10 mm high anhydrous sodium sulphate layer in the front column with 5 mL N - hexane elution activated solid phase extraction.

5 instruments and equipment

5.1 Gas Chromatography-Mass Spectrometer. Negative Chemical Source (NCI). 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 vortex mixer. 5.4 Centrifuge. speed greater than 5 000 r/min. 5.5 nitrogen blowing instrument. 5.6 Rotary evaporator.

6 Preparation and storage of samples

Take about 500g of the sample, the sampling site according to GB 2763 Appendix A implementation, will be forced to stir evenly, into a clean container, Sealed and marked with the mark, and the sample was stored at -18 ° C. During sample and sample preparation, contamination of the sample or changes in the residue content should be prevented.

7 Analysis steps

7.1 Extraction Weigh 2 g sample (accurate to 0.01 g) in 50 mL centrifuge tube, add 10 mL water vortex mixed 1 min, standing 5 min. Join 20 mL of n-hexane acetone (1 1, volume ratio) mixed solvent, vortex mixed for 1 min, centrifuged at 4000 r/min for 3 min, the upper organic Phase transferred into the concentration bottle. Add 10 mL of n-hexane acetone (1 1, volume ratio) mixed solvent, repeat the extraction time, combined The upper organic phase, in 45 ℃ below the water bath under reduced pressure to near dry, to be purified. 7.2 Purification The residue in the concentrated flask was washed twice with 3 mL of n-hexane and transferred to a Florisil solid phase extraction column. With 5 mL of n-hexane The effluent was discarded and eluted with 10 mL of n-hexane + ether (8 + 2, v/v) mixed solvent. The eluate was collected in 10 mL of glass off Tube in the 45 ℃ water bath with nitrogen blowing instrument slowly blowing to near dry, with n-hexane dissolved and set to 0.5mL, gas chromatography-mass spectrometry. 7.3 Determination 7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions A) Column. DB-5ms quartz capillary column, 30 m x 0.25 mm (id) x 0.25 μm, or equivalent; B) column temperature. 50 ℃ for 1 min, at 20 ℃/min heating rate rose to 220 ℃, keep 1 min, The temperature was raised to 250 ° C at a rate of 5 ° C/min and raised to 280 ° C at a rate of 20 ° C/min for 8 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%; flow rate 1.0 mL/min; F) Injection volume. 2 μL; G) Injection method. splitless injection, 1.5 min after the opening valve; H) ionization mode. NCI; I) ionization energy. 184 eV; J) ion source temperature. 150 ° C; K) quadrupole temperature. 150 ° C; L) Reaction gas. methane, purity greater than or equal to 99.99%, reaction gas flow rate. 2 mL/min; M) Measurement method. Select the ion monitoring mode (SIM); N) solvent delay time. 10 min; O) Select the ion measurement. each compound selected a quantitative ion, 2-3 qualitative ions. Each group needs to be measured Sub-according to the peak order, respectively, time points were measured. The retention time of each compound, the quantitative ion, the qualitative ion and the quantitative ion and qualitative The abundance of ions is given in Appendix B. 7.3.2 Quantitative determination According to the content of acaricide in the sample solution, the standard working solution with similar peak area is selected. Standard working solution and sample solution of acaricides The value should be within the linear range of the instrument determination. Standard working solution and sample volume and other volume interspersed injection determination. Under the above chromatographic conditions, 8 species The retention time of the acaricides is given in Appendix B, and the total ion current of the standard is shown in Appendix C, C.1. 7.3.3 Qualitative determination The standard solution and sample solution are determined according to the conditions specified in 7.3.1, if the sample solution and the standard solution in the same retention time peak Now, it is confirmed by mass spectrometry, after deducting the background of the sample spectrum, the selected ions all appear, while the selected ion from the The abundance ratio is consistent with the relative abundance of the ions associated with the standard, and the fluctuation range is within the maximum allowable deviation of Table 1 (see Table 1) The substance is present in the sample. Table 1 Mass Spectrum Relative Ion Abundance Maximum Allowable Deviation Relative ion 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 determination steps.

8 results are calculated and expressed

Use the chromatographic data processing software or calculate the residual content of various acaricides in the sample according to formula (1). A × c × V X = ---------------------- (1) AS x m Where. X. Residue of various acaricides in the sample in milligrams per kilogram (mg/kg); A) the area of various acaricidal agents in the sample solution; C - the concentration of various acaricides in standard working fluid, in micrograms/ml (g/mL); V - Final volume of the final volume in milliliters (mL); AS - standard acupoints in standard working fluids; M - the amount of 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) shall be in accordance with Appendix E 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 F requirements. 10% limit and recovery rate 10.1 Quantitation limits The quantification limit of this method is. 0.01 mg/kg. 10.2 Recovery rate The experimental data on the concentration and recovery of the sample are given in Appendix D.

Appendix A

(Informative) 8 kinds of acaricides pesticides in English generic name, chemical formula, CAS number information Table A.1 8 kinds of acaricides pesticides in English common name, chemical formula, CAS No. information Chinese generic name English generic name chemical molecular formula CAS number Acetylidene Chlorbenside C13H10 Cl2 S 269 103-17-3 Mycobacterium acaricides Quinomethionate C10H6N2OS2 234 2439-01-2 Acetylate Chlorfenson C12H8Cl2O3 S 302 80-33-1 Phytophthora Ethyl Acetone Chlorobenzilate C16H14Cl2O3 324 510-15-6 Bromopropylate C17H16Br2O3 426 18181-80-1 Dicofolone Tetradifon C12H6 Cl4 O2S 354 116-29-0 Pyridaben C19H25ClN2OS 364 96489-71-3

Appendix B

(Informative appendix) Retention time of 8 kinds of acaricides, quantitative ions, qualitative ions and relative abundance Table B.1 Retention times, quantitative ions, qualitative ions and relative abundance of eight acaricides Pesticide name quantitative ion qualitative ion 1 qualitative ion 2 qualitative ion 3 keep time (Min) Acaricides 143 (100) 144 (7.7) 145 (36.1) 13.5 Mycobacterium mites 206 (100) 207 (12.8 208 (11.8) 13.6 Acaricides 175 (100) 176 (8.3) 177 (38.9) 14.0 Lychee mite 223 (100) 224 (16.1) 239 (46.6) 14.6 Ethyl Ester 324 (100) 326 (68.2) 278 (34.5) 262 (40.2) 15.1 Bromide mites 428 (100) 426 (51.) 430 (50.4) 17.5 Diclofenac 320 (100) 318 (75.4) 356 (43.9) 18.1 Pyridaben 217 (100) 219 (39.1) 218 (15.8) 19.8

Appendix C

(Informative) Total ion flow chart of 8 kinds of acaricides standard materials Figure C.1 Total ion chromatogram of eight species of acaricides 1. Acaricidal ether 2. Methylk acaricides 3. Fungicides 4. Lecture dex mite 5 Ethyl ester Mites 4. Bromothylate 7. Diclofenac 8

Appendix D

(Informative) Sample concentration and recovery of the experimental data Table D.1 Experimental data on the concentration and recovery of the sample Pesticide name added concentration (Mg/kg) Recovery rate Precision degree Pesticide name Add concentration (mg/kg) Recovery rate Precision degree Acaricides 0.01 86.7 ~ 112 11.2 ethyl ester acaricides 0.01 77.5 to 113 6.8 0.02 94 to 112 8.6 0.02 84.0 to 104 7.9 0.05 81.2 to 107 9.3 0.05 72.6 to 107 4.5 Methyl killer 0.01 82.1 ~ 118 9.6 Bromo mite 0.01 71.3 ~ 115 13.0 0.02 76.8 to 107 10.2 0.02 78.0 to 114 11.8 0.05 79.4 to 102 7.5 0.05 73.6 to 106 10.8 Acaricidal ester 0.01 79.7 ~ 118 13.1 dicofol 0.01 76.7 to 115 6.9 0.02 85.0 to 110 12.6 0.02 75.0 to 107 7.6 0.05 74.4 to 109 10.8 0.05 74.8 to 108 8.9 Lymanthamidae 0.01 69.1 to 108 14.1 Pyridinidone 0.01 78.2 to 118 8.4 0.02 76.5 to 108 10.6 0.02 75.0 to 109 9.8 0.05 77.4 to 109 13.1 0.05 78.8 to 109 12.3

Appendix E

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

Appendix F

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

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