GB 23200.99-2016 English PDF

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GB 23200.99-2016: Food safety national standard -- Determination of various carbamate pesticide residues in royal jelly by liquid chromatography-mass spectrometry / mass spectrometry
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Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
GB 23200.99-2016	239	Add to Cart	3 days	Food safety national standard -- Determination of various carbamate pesticide residues in royal jelly by liquid chromatography-mass spectrometry / mass spectrometry	Valid

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Basic data

Standard ID: GB 23200.99-2016 (GB23200.99-2016)
Description (Translated English): Food safety national standard -- Determination of various carbamate pesticide residues in royal jelly by liquid chromatography-mass spectrometry / mass spectrometry
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Word Count Estimation: 12,125
Date of Issue: 2016-12-18
Date of Implementation: 2017-06-18
Older Standard (superseded by this standard): SN/T 2572-2010
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 23200.99-2016: Food safety national standard -- Determination of various carbamate pesticide residues in royal jelly by liquid chromatography-mass spectrometry / 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 standard - Determination of various carbamate pesticide residues in royal jelly by liquid chromatography-mass spectrometry/mass spectrometry National Standards of People's Republic of China GB Replace SN/T 2572-2010 National standards for food safety Royal jelly in a variety of carbamate pesticide residues Determination Liquid chromatography - mass spectrometry/mass spectrometry National food safety standards Determination of multiple carbamate pesticides residues in royal-jelly 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 2572-2010 "Import and export royal jelly in a variety of carbamate pesticide residues detection method Liquid chromatography - Mass spectrometry/mass spectrometry ". Compared with SN/T 2572-2010, 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 2572-2010. National standards for food safety Determination of various carbamate pesticide residues in royal jelly Liquid chromatography - mass spectrometry/mass spectrometry

1 Scope

This standard stipulates the royal jelly in the methyl thiouwei, evil worm Wei, isoprocarb, carbamate, methomyl, carbofuran, pirimicarb, Zhong Dingwei residual Amount of liquid chromatography-mass spectrometry/mass spectrometry. This standard applies to royal jelly in the methyl thiouwei, evil worm Wei, isoprene, carbazate, methomyl, carbofuran, pirimicarb, Zhong Dingwei residual The amount of the determination and confirmation, 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 acetonitrile, purified by neutral alumina column chromatography, and analyzed by liquid chromatography-mass spectrometry/mass spectrometry.

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 Methanol (CH4O). Chromatographic purity. 4.1.2 acetonitrile (C2H3N). pure chromatography. 4.1.3 Acetone (C3H6O). Chromatographic pure. 4.1.4 ether (C4H10O). chromatographic purity. 4.1.5 ammonium acetate (CH3COONH4). pure chromatography. 4.1.6 Sodium chloride (NaCl). 4.2 solution preparation 4.2.1 0.005 mol/L ammonium acetate solution. Weigh 0.19 g ammonium acetate dissolved in the amount of water, and then set to 500 mL. 4.2.2 methanol - 0.005 mol/L ammonium acetate solution (6 +4, V/V). take 600 mL of methanol, add 400 mL0.005 mol/L B Ammonium acid solution, shake back spare. 4.2.3 acetone - ether solution (2 8, V/V). take.200 mL of acetone, add 800 mL of ether, shake back. 4.3 standards 4.3.1 carbamate standard products. methyl thiouwei, evil worm Wei, isoprove, carbaryl, carbofuran, pirimicarb, Zhong Dingwei purity ≥ 99.0%. For more than 98.8%, see Appendix A. 4.4 standard solution preparation 4.4.1 urethane standard stock solution. accurately weighed the amount of carbamate standard, dissolved in methanol, were prepared into a concentration of.200 g/mL standard stock solution, 4 ℃ refrigerator storage. 4.4.2 carbamate mixed working solution. according to need, respectively, take appropriate amount of liquid in the same volume bottle, with methanol -0.005 mol/L Ammonium acetate solution was diluted to the appropriate concentration of working solution. Store in 4 ℃ refrigerator. 4.4.3 Preparation of Carbamate Calibration Solution. The standard mixed solution was diluted with a blank sample solution treated with 7.1 and 7.2 to a concentration of 5.0, 10.0, 50.0, 100.0 g/L. Store in 4 ℃ refrigerator. 4.5 Materials 4.5.1 Neutral Alumina Solid Phase Extraction Column (500 mg, 3 mL). Rinse with 5 mL of ether before use.

5 instruments and equipment

5.1 LC-Tandem Mass Spectrometer. Equipped with electrospray ion source and quadrupole mass analyzer. 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 Vortex Mixer. 5.4 Rotary Evaporator. 5.5 Centrifuge. speed greater than 5 000 r/min. 5.6 Solid phase extraction unit with vacuum pump. 5.7 covered plastic centrifuge tube. 50 mL.

6 Preparation and storage of samples

To replace the sample of about 500g, the sampling site according to GB 2763 Appendix A implementation, will be forced to stir evenly, into a clean container sealed, And mark the mark. Save below -18 ° C. During the operation of the sample preparation, the contamination of the sample or the change in the content of the residue should be prevented.

7 Analysis steps

7.1 Extraction Weigh 2 g of sample (accurate to 0.01 g) placed in 50 mL centrifuge tube, add 10 mL water vortex mixed 1 min, standing 5 min. Join 15 mL acetonitrile vortex for 1 min, centrifuged at 4000 r/min for 2 min, transfer the upper solution to 50 mL centrifuge tube. Add the residue Into 2 mL of water and 15 mL of acetonitrile, repeat the extraction time, combined with 2 times the extract, add excess sodium chloride vortex mixing 1 min to 4000 R/min centrifugal 2 min, transfer the upper layer of acetonitrile phase to the concentrated flask, 40 ℃ below the water bath under reduced pressure to near dry, the residue with 3 mL of acetone - ether Mixed solvent dissolved, to be purified. 7.2 Purification The above extract was transferred to a neutral alumina column and the residue was washed three times with 10 mL of acetone-ether mixed solvent. The flow rate is about 1 mL/min. Collect all eluent. 40 ℃ below the water bath concentrated to near dry, with methanol - 0.005 mol/L ammonium acetate The solution was dissolved and set to 4.0 mL, to be determined. 7.3 Determination 7.3.1 Liquid Chromatography - Mass Spectrometry Reference Conditions A) Column. C8, particle size 5 m, 150 mm × 4.6 mm (inner diameter), or equivalent column. B) mobile phase. A. methanol, B. 0.005 mol/L ammonium acetate solution, mobile phase gradient elution program as shown in Table 1. C) Flow rate. 0.3 mL/min. D) Injection volume. 20 μL. E) Column temperature. 20 ° C. F) Scanning mode. positive ion mode. G) Detection method. multiple reaction monitoring. H) aerosol, air curtain gas, auxiliary gas, collision gas are high purity nitrogen; monitoring of ion pairs (m/z) and other reference conditions see Appendix B. Table 1 gradient elution program Time (min) A (%) B (%) 0.00 70 30 8.00 90 10 8.10 100 0 15.00 100 0 15.10 70 30 20.00 70 30 7.3.2 LC/MS-MS determination According to the sample solution to be measured the content of the selected concentration of similar standard calibration solution, test solution to be measured the response value should be detected in the instrument Linear range. Calibration solution and sample solution and other volume injection determination, in the above chromatographic conditions, the chromatogram of carbamate see Appendix C C.1. 7.3.3 Liquid Chromatography - Mass Spectrum Confirmation The retention time of the analyte in the test solution should be determined in the above-mentioned liquid chromatography-tandem mass spectrometry conditions. When the retention time of the solution is corrected The relative abundance of each ion pair in the window should be consistent with the relative abundance of the calibration solution, and the error does not exceed the range specified in Table 2. Table 2 The maximum allowable error of relative ion abundance when qualitative confirmation 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

Use the chromatographic data processor or calculate the amount of carbamate pesticide in the sample by the following formula (1). MΑsi VCsiAi X   .. (1) Where. Xi - Residual content of each carbamate pesticide in the sample in milligrams per kilogram, mg/kg; Ai - the peak area of each carbamate pesticide in the sample solution; V - the final volume of the sample solution, in milliliters, mL; Asi - the peak area of each carbamate pesticide in standard working fluid; Csi - the concentration of each carbamate pesticide in standard working fluid in micrograms per milliliter, g/mL; 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 limit of quantification of carbamate pesticides is 0.01 mg/kg. 10.2 Recovery rate When the concentration of 0.01 mg/kg to 0.05 mg/kg is added to royal jelly, the recovery range is given in Appendix D.

Appendix A

(Informative) 8 kinds of carbamate pesticides in English common name, CAS number, chemical formula, molecular weight information Table A.1 8 kinds of carbamate pesticides in English common name, CAS number, chemical formula, molecular weight information Pesticide generic name English generic name CAS number chemical molecular formula molecular weight Methomyl 16752-77-5 C5H10N2O2S 162 Bugs Bodiocarb 22781-23-3 C11H13NO4 223 Carbofuran 1563-66-2 C12H15NO3 221 Carbaryl 63-25-2 C12H11NO2.201 Pirimicarb 23103-98-2 C11H18N4O2 238 Isoprocarb 2631-40-5 C11H15NO2 193 Secong Wei Fenobucarb 3766-81-2 C12H17NO2 207 Methiocarb 2032-65-7 C11H15NO2S 225

Appendix B

(Informative) API 4000 LC-MS/MS system electrospray ion source reference conditions Monitoring of ion pairs and voltage parameters. A) ion source temperature. 400 ° C; B) electrospray voltage. 5250 V; C) collision air flow rate. 5 L/min; D) air curtain air flow rate. 25 L/min; E) atomization gas flow rate. 55 L/min; F) Auxiliary gas flow rate. 30 L/min. Table B.1 Qualitative/Quantitative Ion Pair, Discharge Voltage (DP), Collision Gas Energy (CE) and Retention Time No. Pesticide Qualitative Ion Pair M/z Quantitative ion pair M/z To cluster voltage DP/V Collision energy CE/V Duration/ms 1 methomyl 163.0/88.1 163.0/106.2 163.0/88.1 43 2 Euphorbia impository 224.1/167.4 224.1/109.2 224.1/167.4 60 3 grams Budweiser 222.1/165.5 222.1/123.1 222.1/165.5 75 4 Carnosilva 202.0/145.2 202.0/127.2 202.1/145.2 60 5 pirimicin 239.1/71.9 239.1/182.4 239.1/71.9 75 6 isopropyl alcohol 194.1/95.0 194.1/137.4 194.1/95.0 60 7 Zhong Dingwei 208.1/94.9 208.1/152.3 208.1/94.9 60 8 methacrylamide 226.1/169.4 226.1/121.1 226.1/169.4 50 Non-commercial statement. The parameters listed in Appendix A are done at the API 4 000 mass spectrometer, where the test instrument model is listed for reference only and does not Commercial purpose, encourage standard users to try different manufacturers and models of equipment.

Appendix C

(Informative) 8 kinds of carbamate standard multi - reaction detection (MRM) chromatograms Figure C.1 Eight carbamate standard multi-reaction detection (MRM) chromatograms

Appendix D

(Informative) Sample concentration and recovery of the experimental data Table D.1 Experimental data on the concentration and recovery of the sample Name of pesticide Add concentration (Mg/kg) Recovery rate% Precision range% Methopius 0.01 70.3 ~ 89.4 13.5 0.02 84.2 to 96.4 10.8 0.05 77.5 to 106 9.6 Viola 0.01 75.1 ~ 96.2 10.2 0.02 85.3 ~ 98.0 4.9 0.05 77.7 to 91.1 12.9 Carbofuran 0.01 78.5 ~ 97.8 10.9 0.02 85.4 ~ 93.7 8.7 0.05 82.7 ~ 93.3 8.5 Carbendazim 0.01 72.6 ~ 97.2 9.3 0.02 93.3 ~ 98.3 5.4 0.05 81.4 to 90.5 6.3 Pirimicin 0.01 73.8 ~ 98.0 8.4 0.02 86.7 to 94.9 9.2 0.05 84.5 to 100 5.1 Isopropyl alcohol 0.01 75.0 to 93.4 9.0 0.02 89.6 ~ 102 7.9 0.05 89.0 to 103 13.1 Zhong Dingwei 0.01 77.7 ~ 95.7 8.5 0.02 97.1 to 114 12.0 0.05 97.2 ~ 103 11.6 Methacillin 0.01 70.9 ~ 89.8 10.8 0.02 85.0 to 101 9.1 0.05 81.8 to 88.2 8.9

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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