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GB 23200.51-2016 English PDF

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GB 23200.51-2016: Food safety national standard -- Determination of dormone residues in food by liquid chromatography-mass spectrometry / mass spectrometry
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GB 23200.51-2016English239 Add to Cart 3 days [Need to translate] Food safety national standard -- Determination of dormone residues in food by liquid chromatography-mass spectrometry / mass spectrometry Valid GB 23200.51-2016

PDF similar to GB 23200.51-2016


Standard similar to GB 23200.51-2016

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Basic data

Standard ID GB 23200.51-2016 (GB23200.51-2016)
Description (Translated English) Food safety national standard -- Determination of dormone residues in food by liquid chromatography-mass spectrometry / mass spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 12,196
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 2231-2008
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 23200.51-2016: Food safety national standard -- Determination of dormone residues in food 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 standards - Determination of dormone residues in food by liquid chromatography - mass spectrometry/mass spectrometry National Standards of People's Republic of China GB Instead of SN/T 2231-2008 National standards for food safety Determination of dormone residues in food Liquid chromatography - mass spectrometry/mass spectrometry National food safety standards- Determination of dinotefuran 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 2231-2008 "Determination of Dicerosperm Residue in Food by Gas Chromatography-Mass Spectrometry". Compared with SN/T 2231-2008, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - the name 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 2231-2008. National standards for food safety Determination of dormone residues in food by liquid chromatography - mass spectrometry/mass spectrometry

1 Scope

This standard specifies the preparation of dendrites in food for import and export and liquid chromatography-mass spectrometry/mass spectrometry. This standard applies to dolomin residues in wheat, peanuts, corn, spinach, apples, carrots, basil leaves, pork and salmon The detection 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 file. 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 sample was extracted with acetonitrile, and the extract was added with anhydrous sodium sulfate. After dehydration, the graphitized non-porous carbon column (Envi-Carb)/amidopropyl Silica-based silica gel column (LC-NH2) purification, liquid chromatography-mass spectrometry/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 sodium chloride (NaCl). excellent grade pure. 4.1.6 anhydrous sodium sulfate (Na2SO4). analysis of pure, 650 ℃ burning 4 h, after natural cooling stored in a sealed bottle in reserve. 4.1.7 Potassium hydrogen phosphate (K2HPO4). analytical grade. 4.1.8 Potassium dihydrogen phosphate (KH2PO4). Analytical purity. 4.1.9 Sodium hydroxide (NaOH). Analytical purity. 4.1.10 hydrochloric acid (HCl). excellent grade pure. 4.2 solution preparation 4.2.1 1 mol/L Sodium hydroxide. Weigh 40 g of sodium hydroxide and dissolve in 1 L of water. 4.2.2 1 mol/L hydrochloric acid. Weigh 36.5 g of pure hydrochloric acid and dissolve in 1 L of water. 4.2.3 N-Hexane Saturated Alice. 100 mL of acetonitrile and 100 mL of n-hexane were added to the 250 mL separatory funnel, The bottom layer is n-hexane saturated acetonitrile. 4.2.4 Acetone-n-Hexane (1 1, V/V). Mix an equal volume of acetone and n-hexane to shake well. 4.2.5 Phosphate buffer. 0.5 mol/L (pH = 7.0), weigh 52.7 g of dipotassium hydrogen phosphate and 30.2 g of potassium dihydrogen phosphate, add about 500 mL Water dissolved, with 1 mol/L sodium hydroxide or 1 mol/L hydrochloric acid to adjust pH7.0, add water to volume 1 L. 4.3 standards 4.3.1 Dinotefuran reference substance. (dinotefuran, C7H14N4O3), CAS NO. 165252-70-0, purity greater than or equal to 98%. 4.4 standard solution preparation 4.4.1 Dipyrazole standard stock solution. Weigh the appropriate amount of dinotefuran standard, with acetone - n-hexane (1 1, V/V) prepared into 1.0 mg/mL standard Quasi-stock solution; 0 ~ 4 0C save. The shelf life is one year. 4.4.2 Dipyrazole standard working solution. Prepare the stock solution with acetone-n-hexane (1 1, V/V) to form a suitable concentration Working fluid. 0 ~ 4 0C save. The shelf life is one month. 4.5 Materials 4.5.1 Envi-Carb/LC-NH2 solid phase extraction column. 500 mg/500 mg. Supelclean ENVI-Carb SPE9 (Graphitized non-porous Carbon) in series with Supelclean LC-NH2 SPE (amide propylsilylated silica gel). 4.5.2 Filtration. 0.2 μm.

5 instruments and equipment

5.1 Liquid Chromatography-Mass Spectrometry/Mass Spectrometer. Equipped with an electrospray ion source (ESI). 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 whirlpool mixer. 5.4 Rotary Evaporator. 5.5 high speed homogenizer. 10000 r/min. 5.6 Centrifuge. 5.7 Centrifuge tube. 100 mL. 5.8 separatory funnel. 250 mL, 150 mL. 5.9 Grain grinder. 5.10 Food mashing machine. 5.11 Peanut Crusher. 5.12 oscillator.

6 Preparation and storage of samples

6.1 Preparation of the sample 6.1.1 Wheat, corn 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, vegetables, fish, meat 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 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, peanut samples stored at 0 ~ 4 ℃; fish, meat and fruits and vegetables samples frozen at -18 ℃ below the sample. 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 Wheat, corn, peanuts Weigh 5 g of sample (accurate to 0.01 g) in a 100 mL centrifuge tube and add 20 mL of water for 5 min. Add 30 mL of acetonitrile to 10,000 R/min homogeneous extraction 1 min, centrifugation 3 min, the extract was filtered to 250 mL separatory funnel, the residue and then 20 mL of acetonitrile repeated extraction of a Times. The combined extracts were added to a separatory funnel and 20 g of sodium chloride and 60 mL of phosphate buffer were added successively to shake for 3 min. After standing, discard the water Floor. Acetonitrile layer by adding 5 g of anhydrous sodium sulfate dehydration at 40 ° C after rotation concentrated to near dry. 7.1.2 fruits, vegetables Weigh 10 g sample (accurate to 0.01 g) in 100 mL centrifuge tube, add 30 mL of acetonitrile, at 10000 r/min homogeneous extraction 1 min, After centrifugation for 3 min, the extract was filtered into a 250 mL separatory funnel and the residue was extracted again with 20 mL of acetonitrile. The combined extracts were separated Funnel, followed by adding 20 g of sodium chloride and 60 mL of phosphate buffer, shaking 3 min. After standing, discard the water layer. Acetonitrile layer added 5 g no Sodium sulfate dehydration after 40 ° C rotation concentrated to near dry. 7.1.3 Fish and meat Weigh 10g sample (accurate to 0.01 g) in 100 mL centrifuge tube, add 30 mL of acetonitrile, whirlpool mixed evenly after ultrasonic extraction 15 min, centrifuged 3 min, the extract was filtered into a 250 mL separatory funnel, and the residue was extracted again with 20 mL of acetonitrile. Merge extraction Liquid in a separatory funnel, followed by adding 20 g of sodium chloride and 60 mL of phosphate buffer, shaking 3 min. After standing, discard the water layer. Acetonitrile layer plus Into 5 g anhydrous sodium sulfate after dehydration at 40 ° C rotation concentrated to near dry. 7.2 Purification 7.2.1 Wheat, corn, peanuts, fish, meat The extract was dissolved in 20 mL of n-hexane and transferred to a 150 mL separatory funnel and dissolved with 20 mL of n-hexane saturated acetonitrile Liquid extraction 2 times, take the next solution to join the extract, 40 ℃ under reduced pressure concentrated dry, add 2 mL of acetonitrile dissolved. Envi-carb/LC-NH2 (500 mg/500 mg) was pre-eluted with 10 mL of acetonitrile and the effluent was discarded. The above obtained solution was poured, And rinsed with 20 mL of acetonitrile. The eluate was collected and concentrated to near dryness at 40 ° C. The residue was dissolved in 2.0 mL of acetonitrile and passed through 0.2 μm Membrane for liquid chromatography - mass spectrometry. 7.2.2 vegetables, fruits Envi-carb/LC-NH2 (500 mg/500 mg) was pre-eluted with 10 mL of acetonitrile and the effluent was discarded. The above obtained solution was poured, And rinsed with 20 mL of acetonitrile. The eluate was collected and concentrated to near dryness at 40 ° C. The residue was dissolved in 2.0 mL of acetonitrile and passed through 0.2 μm Membrane for liquid chromatography - mass spectrometry. 7.3 Determination 7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions A. Column. Waters Acquity Uplc BEH C8 1.7 μm B. Mobile phase. water (A) acetonitrile (B) gradient Table 1 Mobile phase gradient Time/min flow rate/mL/min% A% B 0.00 0.25 60 40 0.30 0.25 60 40 2.00 0.25 30 70 2.50 0.25 60 40 C. Column temperature. 30 ° C. D. Flow rate. 0.2 mL/min. E. Injection volume. 10 μL. F. Running time. 3.5 min G. Mass spectrometry conditions See Appendix A. 7.3.2 Determination and confirmation of chromatography According to the content of the sample in the sample, the selected concentration of similar standard working solution, the standard working solution and sample solution volume into the sample Determination of the standard working solution and the sample solution of dindue in the response of the instrument should be within the linear range. If the sample is in the mass chromatogram of the standard working solution, the chromatographic peaks appear at the same retention time, and the selected ions appear. The abundance ratio of the selected ions is proportional to the abundance ratio of the corresponding ions of the standard, and the value is within the allowable range (see Table 1 for the allowable range). In condition 7.3.1 , The retention time of dinotefuran is 0.6 min. Under the condition of 7.3.1, the spectrum of the dinotefuran standard is shown in Appendix B. Table 2 Use Qualitative Liquid Chromatography - Mass Spectrometry Relative Ion Abundance Maximum Allowable Deviation Relative ion abundance > 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 dinotefuran residues in the sample according to formula (1). A × c × V AS x m (1) Where. X - Diclofenac residues in the sample, in micrograms per kilogram (μg/kg); A - peak area of dinotefuran in sample solution; C - the concentration of the standard solution of dwarf pesticide is in micrograms per liter (μg/L); V - the final volume of the sample solution in milliliters (mL); AS - the peak area of the standard working solution of dwarfazapine; 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 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 quantification limit of this method was 10 μg/kg. 10.2 Recovery rate The experimental data on the concentration and recovery of the sample are given in Appendix C.

Appendix A

(Informative) Table A.1 Mass spectrometry conditions Table A.2 Multi-reaction monitoring conditions Note. Add "*" ions for quantitation. Non-Commercial Notices. The parameters listed in Appendix A are performed on a Waters Quattro Premier mass spectrometer, where the test instrument model Only to provide a reference, does not involve commercial purposes, to encourage standard users to try to use different manufacturers or models of equipment. Ionization mode ESI Capillary voltage 3.0 kV The source temperature is 120 ° C The solvent temperature was 350 ° C Taper hole air nitrogen, 50L/h Solvent gas stream nitrogen, 600 L/h Collision air pressure argon, 3.10 × 10-6 Pa Monitoring mode multiple reaction monitoring Compound ion ion ion residence time cone hole voltage collision energy Dinoprams 202.9 128.8 * 0.10 s 20 V 12 eV 156.8 0.10 s 20 V 10 eV

Appendix B

(Informative) Standard substance chromatogram Figure B.1 Damp Fungus Liquid Chromatography-Mass Spectrometry/Mass Spectrometry Multi-Reaction Monitoring Chromatogram

Appendix C

(Informative) Sample concentration and recovery of the experimental data Table C.1 Experimental data on the concentration and recovery of the sample sample name Add concentration (Μg/kg) Recovery rate(%) peanut 10 67.57% 20 74.17% 40 82.68% corn 10 73.27% 20 80.33% 40 83.19% wheat 10 68.50% 20 74.23% 40 81.81% Basil 10 76.55% 20 83.03% 40 89.17% pork 10 70.77% 20 79.76% 40 84.73% spinach 10 79.83% 20 83.40% 40 88.16% Salmon 10 72.20% 20 80.18% 40 87.94% apple 10 78.53% 20 82.36% 40 87.07%

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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