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GB 23200.94-2016 English PDF

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GB 23200.94-2016: Food safety national standard -- Determination of Trichlorfon, Dichlorvos and Phytophthora Phosphorus Residues in Animal Foods by Liquid Chromatography-Mass Spectrometry / Mass Spectrometry
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GB 23200.94-2016English239 Add to Cart 3 days [Need to translate] Food safety national standard -- Determination of Trichlorfon, Dichlorvos and Phytophthora Phosphorus Residues in Animal Foods by Liquid Chromatography-Mass Spectrometry / Mass Spectrometry Valid GB 23200.94-2016

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Basic data

Standard ID GB 23200.94-2016 (GB23200.94-2016)
Description (Translated English) Food safety national standard -- Determination of Trichlorfon, Dichlorvos and Phytophthora Phosphorus Residues in Animal Foods by Liquid Chromatography-Mass Spectrometry / Mass Spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 12,167
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 1920-2007
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 23200.94-2016: Food safety national standard -- Determination of Trichlorfon, Dichlorvos and Phytophthora Phosphorus Residues in Animal Foods by Liquid Chromatography-Mass Spectrometry / Mass Spectrometry



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Food safety national standard - Determination of Trichlorfon, Dichlorvos and Phytophthora Phosphorus Residues in Animal Foods by Liquid Chromatography-Mass Spectrometry/Mass Spectrometry National Standards of People's Republic of China GB Instead of SN/T 1920-2007 National standards for food safety Animal-derived food trichlorfon, dichlorvos, Determination of Phosphorus Residue in Liquid chromatography - mass spectrometry/mass spectrometry National food safety standards- Determination of trichlorfon, dichlorvos and coumaphos residues in animal-derived 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 1920-2007 "detection method of trichlorfon, dichlorvos and levophos residues in animal-derived foodstuffs Liquid chromatography-mass spectrometry/mass spectrometry ". Compared with SN/T 1920-2007, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - the standard name "import and export animal food" to "animal food"; - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN/T 1920-2007. National standards for food safety Determination of trichlorfon, dichlorvos and levophos residues in animal - derived foods Liquid chromatography - mass spectrometry/mass spectrometry

1 Scope

This standard specifies the sample preparation and liquid chromatography for the residues of trichlorfon, dichlorvos, and leopophylla in livestock, poultry flesh, salted casings and honey Method of mass spectrometry/mass spectrometry. This standard applies to the separation of meat, salted casings and honey trichlorfon, dichlorvos, flies phosphorus phosphorus residue determination, other food can refer to carried out.

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

Samples of trichlorfon, dichlorvos, flies toxic phosphorus extracted with dichloromethane or ethyl acetate, the extract is concentrated, degreasing, with liquid color Spectrum - mass spectrometry/mass spectrometry, external standard area method quantitative, sub - ion abundance ratio qualitative.

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 4.1.2 acetonitrile (CH3CN). high performance liquid chromatography grade. 4.1.3 Methanol (CH3OH). High performance liquid chromatography grade. 4.1.4 Ethyl acetate (C4H8O2). 4.1.5 Bichloromethane (CH2Cl2). 4.1.6 Cyclohexane (C6H12). 4.1.7 sodium sulfate (Na2SO4). 650 ℃ burning 4 h, in the dryer to cool to room temperature, stored in a sealed bottle in reserve. 4.1.8 ammonium acetate (CH3COONH4). excellent grade pure or equivalent. 4.2 solution preparation 4.2.1 50 mmol/L ammonium acetate solution. Weigh 0.385 g of ammonium acetate in 1 000 mL of water 4.3 standards 4.3.1 Trichlorfon (CAS. 52-68-6, Molecular formula. C4H8Cl3O4P) Standard. purity ≥ 98.0%. 4.3.2 dichlorvos (Dichlorvos, CAS. 62-73-7, molecular formula. C4H7Cl2O4P) standard. purity ≥ 97.6%. 4.3.3 Flamingophos (Coumaphos, CAS. 56-72-4, Molecular formula. C14H16ClO5PS) Standard. Purity ≥99.9%. 4.4 standard solution preparation 4.4.1 standard stock solution. respectively, accurately weighed appropriate trichlorfon, dichlorvos, flies phosphorus standard, with methanol prepared into a concentration of 100 μg/mL Concentration of mixed standard stock solution. The solution in 0 ℃ ~ 4 ℃ refrigerator in the dark, can be used for 3 months. 4.4.2 blank sample extract. with no trichlorfon, dichlorvos, flies phosphorus phosphorus residue samples, according to 7.1 prepared blank sample extract. 4.4.3 Standard working solution. Standard stock solution is diluted to 50 ng/mL, 100 ng/mL,.200 Ng/mL, 500 ng/mL mixed standard working solution. Placed in 0 ℃ ~ 4 ℃ refrigerator in the dark, can be used for 3 days.

5 instruments and equipment

5.1 High Performance Liquid Chromatography - Mass Spectrometry/Mass Spectrometer. Triple Quadrupole Mass Spectrometer, Distribution Spray Ion Source (ESI) or equivalent. 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 Ultrasonic cleaner. 5.4 Vortex Mixer. 5.5 Rotary Evaporator. 5.6 Centrifuge. 5000 r/min. 5.7 homogenizer. 5.8 0.45 μm microporous membrane.

6 Preparation and storage of samples

6.1 Preparation of the sample 6.1.1 Split meat Take a typical sample of about 500 g, broken with a tissue crusher, into a clean container as a sample, sealed and labeled. 6.1.2 casing Take a representative sample of about 100 g, cut with scissors to less than 2 mm, into a clean container as a sample, sealed and labeled. 6.1.3 honey Take a representative sample of about 500 g, stir evenly into the clean container sealed and do a good job. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 6.2 Sample storage Split meat, casings, honey and other samples in -18 ℃ below the frozen storage. 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 and purification 7.1.1 Split meat A) accurately weighed 5 g homogeneous sample (accurate to 0.01 g) in 50 mL stopper tube, add 5 g of anhydrous sodium sulfate to mix, add Into 15 mL of dichloromethane, homogenizer (10000 r/min) homogeneous 2 min, 4 000 r/min centrifugal 3 min, the organic phase to Transferred to 100 mL pear-shaped distillation bottle, the residue and then 2 × 10 mL dichloromethane homogeneous extraction twice. B) The organic phases were combined by centrifugation and evaporated to 2 mL at 40 ° C. The sample was transferred to a 5 mL graduated tube and washed with a small amount of dichloromethane Wash the pear-shaped distillation bottle, combine the washing liquid to the scale tube, room temperature nitrogen concentrated to dry. Quantitative addition of 1.0 mL of acetonitrile dissolved After adding 2 mL of cyclohexane vortex for 2 min, centrifuge at 2 500 r/min for 3 min and add the lower acetonitrile to 0.45 μm Microporous membrane, for liquid chromatography - mass spectrometry/mass spectrometry. 7.1.2 casing Accurately weighed 5 g sample (accurate to 0.01 g) in 50 mL stoppered centrifuge bottle, add 2 g of anhydrous sodium sulfate mix, then add 15 mL Dichloromethane, covered with a lid and placed in an ultrasonic cleaner for 30 min. After cooling, the organic phase was transferred to 100 mL of pear-shaped distillation Bottle, the residue and then 2 × 10 mL with dichloromethane mixed ultrasonic extraction twice, centrifugal organic phase. Next, follow the "Centrifugal" in 7.1.1 Merge organic phase "after the steps. 7.1.3 honey Weigh 5 g of sample (accurate to 0.01 g) in 50 mL stoppered centrifuge tube, add 10 mL of water, add 25 mL of ethyl acetate, mix in vortex And the mixture was centrifuged at 3 000 r/min for 5 min. The upper layer of ethyl acetate extract was collected in a concentrated flask and the residue was further added to 20 mL Ethyl acetate, the above procedure was repeated and the ethyl acetate extraction solution was combined. Concentrated to about 3 mL under reduced pressure at 50 ° C and transferred to 10 mL centrifugation Tube, with 5 mL of ethyl acetate in two batches of concentrated bottles, combined washing solution in a centrifuge tube, dry with nitrogen. Add 1.0 mL of acetonitrile to dissolve residue Slag and pass through a 0.45 μm microporous membrane for liquid chromatography-mass spectrometry/mass spectrometry. 7.2 Determination 7.2.1 Liquid Chromatography - Mass Spectrometry/Mass Spectrometry Reference Conditions A) Column. Column packed with octadecyl silane bonded phase column, 4.6  150 mm, 5 μm or equivalent; B) Mobile phase. methanol. 50 mmol/L ammonium acetate, gradient elution procedure See Appendix A; C) Flow rate. 0.50 mL/min or optimized according to instrument conditions; D) Column temperature. 40 ° C; E) Injection volume. 10 μL; F) ion source. electrospray ion source; G) Scanning mode. positive ions; H) Detection methods. multiple reaction monitoring (MRM); I) Mass Spectrometry/Mass Spectrometry Refer to Appendix B for reference conditions 7.2.2 Chromatographic determination and confirmation The sample solution and standard working solution were determined according to 7.2.1 liquid chromatography-mass spectrometry/mass spectrometry conditions. The external standard method was used to determine the enemy Insects, dichlorvos, flies phosphorus residues. Residue of the sample to be measured in the sample should be within the standard curve, if the residue exceeds the standard curve And the blank sample extract is used for proper dilution. In the above chromatographic conditions, trichlorfon, dichlorvos, flies phosphorus phosphorus quality peak protection The time is about 13.2 min, 14.1 min, 15.9 min. The multi-reaction monitoring chromatogram of the standard is shown in Figure C.1 in Appendix C. Under the same experimental conditions, the relative retention time of the sample and the mass chromatographic peak of the test substance in the standard working fluid was within 2.5%, and In the sample quality chromatogram after subtracting the background, the selected pair of ions appears, and the relative abundance of the standard is not allowed to exceed Table 1 specified range, you can determine the existence of the corresponding sample in the sample. Table 1 Maximum Adsorption Error for Relative Ion Abundance Using Qualitative Liquid Chromatography-Mass Spectrometry/Mass Spectrometry Relative ion abundance > 50% > 20% to 50% > 10% to 20% ≤10% Maximum permissible deviation ± 20% ± 25% ± 30% ± 50% 7.3 blank experiment In addition to the sample, according to the above determination steps.

8 results are calculated and expressed

Using the external standard method of data processing software, or drawing the standard curve, according to formula (1) calculated samples of trichlorfon, dichlorvos, flies phosphorus The amount of residue. 1000   VC X (1) Where. x - the amount of trichlorfon, dichlorvos and flies in the sample, in milligrams per kilogram (mg/kg); C - Concentration of trichlorfon, dichlorvos and flies in the sample from the standard curve, in ng/ml (ng/mL); V - the final volume of the sample solution in milliliters (mL); 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) 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 determination of trichlorfon, dichlorvos and flies were 0.010 mg/kg. 10.2 Recovery rate 10.2.1 Concentration and recovery of trichlorfon in casings Data. When the concentration was 0.010 mg/kg, the recoveries ranged from 73.0% to 94.0% When the concentration was 0.020 mg/kg, the recoveries ranged from 78.0% to 95.0% When the concentration was 0.040 mg/kg, the recovery was between 78.0% and 95.0%. 10.2.2 Addiction concentration and recovery rate of dichlorvos in casings Data. When the concentration was 0.010 mg/kg, the recoveries ranged from 76.0% to 98.0% When the concentration was 0.020 mg/kg, the recoveries ranged from 78.0% to 98.0% When the concentration was 0.040 mg/kg, the recoveries ranged from 86.0% to 95.0%. 10.2.3 Concentration and recovery of poisonous phosphorus in casings. When the concentration was 0.010 mg/kg, the recoveries ranged from 75.0% to 95.0% When the concentration was 0.020 mg/kg, the recoveries ranged from 80.0% to 96.0% When the concentration was 0.040 mg/kg, the recoveries ranged from 77.0% to 92.0%. 10.2.4 Concentration and recovery of trichlorfon in divided meat Data. When the concentration was 0.010 mg/kg, the recoveries ranged from 92.0% to 115% When the concentration was 0.020 mg/kg, the recoveries ranged from 86.5% to 113% When the concentration was 0.040 mg/kg, the recovery was between 80.8% and 101%. 10.2.5 Add the concentration of dichlorvos in the divided meat and its recovery rate Data. When the concentration was 0.010 mg/kg, the recoveries ranged from 93.0% to 110% When the concentration was 0.020 mg/kg, the recoveries ranged from 88.5% to 108% When the concentration was 0.040 mg/kg, the recovery was between 84.3% and 110%. 10.2.6 Concentration and recovery of poisonous phosphorus in divided meat. When the concentration was 0.010 mg/kg, the recoveries ranged from 91.0% to 112% When the concentration was 0.020 mg/kg, the recoveries ranged from 79.0% to 102% When the concentration was 0.040 mg/kg, the recoveries ranged from 73.9% to 95.3%. 10.2.7 Concentration and recovery of trichlorfon in honey Data. When the concentration was 0.010 mg/kg, the recoveries ranged from 70.0% to 110% When the concentration was 0.020 mg/kg, the recoveries ranged from 79.0% to 104% When the concentration was 0.040 mg/kg, the recovery was between 80.0% and 107%. 10.2.8 Additive concentration of honey dichlorvos and its recovery rate Data. When the concentration was 0.010 mg/kg, the recoveries ranged from 70.0% to 92.0% When the concentration was 0.020 mg/kg, the recoveries ranged from 71.0% to 91.0% When the concentration was 0.040 mg/kg, the recoveries ranged from 70.0% to 96.0%. 10.2.9 Concentration and recovery of poisonous phosphorus in honey. When the concentration was 0.010 mg/kg, the recoveries ranged from 79.0% to 110% When the concentration was 0.020 mg/kg, the recoveries ranged from 74.0% to 105% When the concentration was 0.040 mg/kg, the recovery was between 71.0% and 104%.

Appendix A

(Informative) Gradient elution reference conditions Table A.1 Mobile phase gradient elution program Time/min methanol/(%) 50 mmol/L ammonium acetate/(%) 0 10.0 90.0 5.00 10.0 90.0 10.00 95.0 5.0 18.00 95.0 5.0 18.01 10.0 90.0 25.00 10.0 90.0

Appendix A

(Informative) API 4000 LC-MS/MS system for detection of trichlorfon, dichlorvos, flies phosphorus reference conditions A.1 API 4000 LC-MS/MS System Electrospray Ion Source Reference Conditions Monitoring of ion pairs and voltage parameters. A) Curtain gas (CUR). 15.00 Pa; B) Atomizing gas (GS1). 40.00 Pa; C) Auxiliary heated gas (GS2). 45.00 L/min; D) collision gas (CAD). 7.00 Pa; E) Ion source nebulizer voltage (IS). 5000.00 V; F) spray needle temperature. (TEM). 550.00 ° C; G) Qualitative ion pair, quantitative ion pair, de-cluster voltage, collision energy, collision chamber outlet voltage See Table B.1. Table B.1 Qualitative ion pairs, Quantum ion pairs, Cladding voltage, Collision energy, and collision chamber outlet voltage To be measured Q1 M/z Q3 M/z To cluster voltage Collision energy Collision chamber outlet voltage Trichlorfon Trichlorfon 259.0a 109.2 63.0 26.5 19.0 256.9 221.2 63.0 16.0 13.0 Dichlorvos Dichlorvos 221.3 a 109.2 63.0 25.5 19.0 223.3 109.0 63.0 25.0 18.0 Flies phosphorus Coumafos 363.3 a 307.0 96.0 25.0 20.0 363.3 227.0 96.0 36.0 13.0 A is a quantitative ion pair.

Appendix B

(Informative) B.1 Standard multi-reaction monitoring chromatogram Figure C..1 Trichlorfon, dichlorvos, flies toxic phosphorus standard solution multi-reaction monitoring chromatogram * Non-commercial statement. The equipment and models used in this standard do not involve commercial purposes, encourage standard messengers to try different manufacturers or models of equipment.

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

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