GB 23200.104-2016 English PDF

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GB 23200.104-2016: Food safety national standard -- Meat and meat products -- Determination of 2-methyl-4-chloro and 2-methyl-4-chlorobutyric acid residues by liquid chromatography-mass spectrometry
Status: Valid

Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
GB 23200.104-2016	219	Add to Cart	3 days	Food safety national standard -- Meat and meat products -- Determination of 2-methyl-4-chloro and 2-methyl-4-chlorobutyric acid residues by liquid chromatography-mass spectrometry	Valid

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Basic data

Standard ID: GB 23200.104-2016 (GB23200.104-2016)
Description (Translated English): Food safety national standard -- Meat and meat products -- Determination of 2-methyl-4-chloro and 2-methyl-4-chlorobutyric acid residues by liquid chromatography-mass spectrometry
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Word Count Estimation: 11,118
Date of Issue: 2016-12-18
Date of Implementation: 2017-06-18
Older Standard (superseded by this standard): SN/T 1392-2004
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 23200.104-2016: Food safety national standard -- Meat and meat products -- Determination of 2-methyl-4-chloro and 2-methyl-4-chlorobutyric acid residues by liquid chromatography-mass spectrometry

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Food safety national standard - Meat and meat products - Determination of 2-methyl-4-chloro and 2-methyl-4-chlorobutyric acid residues by liquid chromatography-mass spectrometry ICS National Standards of People's Republic of China GB Instead of SN/T 1392-2004 National standards for food safety Meat and meat products in the 2 a 4 chlorine and 2 a 4 chlorobutyric acid residue Determination of the amount of retention Liquid chromatography - mass spectrometry National food safety standards- Determination of MCPA and MCPB residues in meat and meat products 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 1392-2015 "Method for the determination of 2-methyl-4-chloro and 2-chlorobutyric acid residues in meat and meat products for liquid chromatography / Tandem mass spectrometry ". This standard compared with SN/T 1392-2015, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - the name of the "export of meat and meat products" to "meat and meat products"; - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN/T 1392-2004; -SN/T 1392-2015. National standards for food safety Determination of 2 - 4 - chloro and 2 - 4 - chlorobutyric acid residues in meat and meat products Liquid chromatography - mass spectrometry

1 Scope

This standard specifies the method for the determination of 2-methylchloride and 2-methylchlorobutyric acid residues in meat and meat products by liquid chromatography-mass spectrometry. This standard applies to the export of frozen frozen beef, fish, pork, chicken, beef canned 2 a 4 chlorine and 2 a 4 chlorobutyric acid residues Detection, 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

Under acidic conditions, the residual 2-methyl-4-chloro, 2-methyl-4-chlorobutyric acid in the sample was extracted with methylene chloride, and the extract was replaced with solvent. 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 dichloromethane (CH2Cl2). chromatographic purity. 4.1.2 Methanol (CH3OH). Chromatographic Purification. 4.1.3 Formic acid (HCOOH). Chromatographic pure. 4.1.4 concentrated sulfuric acid (H2SO4). excellent grade pure. 4.1.5 sodium chloride. excellent grade pure. 4.2 solution preparation 4.2.1 Sulfuric acid - water (19, V/V). take 100 mL concentrated sulfuric acid, add 900mL of water, shake back. 4.2.2 0.1% formic acid aqueous solution. take 1 mL of formic acid, the volume of water to 1000 mL. 4.3 standards 2 a 4 chlorobutyric acid standard. purity ≥ 99%, CAS. 94-82-6. 4.4 standard solution preparation 4.4.1 0.1 mg/mL standard stock solution. accurately weighed the appropriate amount of 2 a 4 chlorine, 2 a 4 chlorobutyric acid standard, with methanol prepared into the concentration Prepare the solution for 0.1 mg/mL standard. Store in 4 ℃ refrigerator. 4.4.2 mixed standard working fluid. the use of the corresponding matrix solution prepared with the appropriate concentration of the standard working solution, stored in 4 ℃ refrigerator.

5 instruments and equipment

5.1 Ultra High Pressure Liquid Chromatography - Tandem Mass Spectrometer with Electrospray Ion Source (ESI). 5.2 high-speed homogenizer. not less than 12000 r/min. 5.3 Centrifuge. not less than 4000 r/min. 5.4 Analytical balance. 0.01 g and 0.0001 g. 5.5 nitrogen blowing instrument. 5.6 Scroll Mixer.

6 Preparation and storage of samples

6.1 Preparation of the sample Take a representative sample 500g, sample sampling site according to GB 2763 Appendix A implementation, crushing machine, and then ground into fine powder Shaped, packed into a clean glass container, sealed and marked. 6.2 Sample storage The samples were cryopreserved at -18 ° C.

7 Analysis steps

7.1 Extraction and purification Weigh the sample 4 g (accurate to 0.01 g) in a 50 mL centrifuge tube, add 3 mL of methanol, 1 mL of sulfuric acid-water, 2 g of sodium chloride and 20 mL Dichloromethane. In the high-speed homogenizer on the homogeneous extraction 2 min, centrifugation, take the supernatant in another centrifuge tube, standing, take the next layer of dichloromethane Layer 10 mL. Repeat the extraction once, merge the two extracts, at 40oC nitrogen blowing near dry, with methanol volume to 2 mL, vortex, membrane, for Determination of Ultra - High Pressure Liquid Chromatography by Tandem Mass Spectrometry. 7.2 Determination 7.2.1 Liquid Chromatographic Reference Conditions A) Column. C18, 1.8 μm, 2.1 x 50 mm or equivalent; B) 0.1% formic acid aqueous solution of methanol, gradient elution see Table 1; C) Flow rate. 0.5 mL/min; D) Injection volume. 5 μL; E) Column temperature. room temperature; Table 1 Liquid Chromatography Gradient Elution Procedure Time (min) 0.1% Formic acid Aqueous solution (%) Methanol (%) 7.2.2 Mass spectrometry reference conditions A) ion source. electrospray ion source B) Scan mode. negative ion mode C) Detection method. Multiple reaction monitoring MRM D) the rate. the unit mass resolution E) Refer to A.1 for other reference mass spectrometry conditions 7.2.3 Chromatographic determination and confirmation According to the determined liquid chromatography - tandem mass spectrometry conditions, the sample and blank matrix plus standard working solution, the response value should be detected in the instrument In the linear range, the peak area of the chromatogram was quantified by the external standard method, and the negative ion mode was scanned. Under the above chromatographic conditions, 2-methyl-4-chloro and 2-methyl-4-chlorobutyric acid Of the retention time of about 1.90 min and 2.10 min. 2 Selective ion flow chart of the standard solution of methyl 4-chloro and 2-chlorobutyric acid is shown in Appendix B.1 and attached Record B.2. If the sample solution with the standard working solution in the selective ion chromatogram at the same retention time there is a chromatographic peak that can be produced according to the two Group of ions between the abundance ratio, to confirm it. Under the same experimental conditions, the retention time of the test substance in the sample and the corresponding working solution in the standard retention time deviation of ± 2.5% And the relative abundance of the qualitative ions of each component in the sample spectrum and the relative abundance of the qualitative ions in the standard working solution are not allowed When the range specified in Table 2 is specified, it may be determined that such a test substance is present in the sample. The maximum allowable error of relative ion abundance when using gas chromatography - mass spectrometry 7.3 blank test Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10% Permissible relative deviations ± relative relative to ± relative relative permissible relative permissible Except for the addition of samples, according to the above conditions and procedures for determination.

8 results are calculated and expressed

The residual value of 2-methyl-4-chloro and 2-methyl-4-chlorobutyric acid in the sample was calculated by the chromatographic data processing system or the formula (1). X - the amount of 2-methylchloride and 2-methyl-4-chlorobutyric acid in the sample, in milligrams per kilogram, mg/kg A - the peak area of 2 - 4 - chloro and 2 - methyl - 4 - chlorobutyric acid in the sample solution; V - the final volume of the sample, in milliliters, mL; The peak area of the standard working solution of As - 2 - 4 - chloro and 2 - methyl - 4 - chlorobutyric acid; C - 2 methyl 4 - chloro and 2 - methyl - 4 - chlorobutyric acid standard working solution in micrograms per milliliter, g/mL; M - the final sample quality of the 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 reproducible conditions and their arithmetic mean (percentage) shall be in accordance with the Record 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 the Record the requirements of D. 10% limit and recovery rate 10.1 Quantitation limits The quantitative line of this method is. 0.01 mg/kg. 10.2 Recovery rate In the beef, pork sausage, fish, chicken and beef canned samples were added 2 a 4 chlorine, 2 a 4 chlorobutyric acid, add the concentration and its back The yield is given in Appendix E.

Appendix A

(Informative) Mass spectrometry parameters A. Liquid Chromatography-Mass Spectrometry/Mass Spectrometry Parameters A) Air curtain gas pressure (CUR). 15 Psi (nitrogen); B) Ion source spray voltage (IS). - 4500V; C) atomization temperature (TEM). 550 oC; D) Atomizing gas pressure (GAS1). 55 Psi (nitrogen); E) Heating auxiliary gas (GAS2). 80 Psi (nitrogen); F) collision air flow ratio (CAD). 7; G) other parameters in Table A. Table A MCPA and MCPA Select ion and mass spectrometry parameters No. Compound Reference Retention Time Qualitative Ion Pair Discharge Voltage (DP)/V Collision Gas Energy (CE)/V * For quantitative ion pairs 1) Non-commercial notices. The parameters listed in A are done on the API 4000 Plus mass spectrometer/mass spectrometer. The experimental instruments listed here are for the purpose of providing Test, does not involve commercial purposes, to encourage standard users to try different models of equipment.

Appendix B

(Informative) Figure B.1 MCPA Standard LC-MS/MS MRM Chart Figure B.2 MCPB Standard LC-MS/MS MRM Chart

Appendix C

(Normative appendix) Laboratory repeatability requirements Table C.1 Laboratory repeatability requirements Measured component content

Appendix D

(Normative appendix) Inter-laboratory reproducibility requirements Table D.1 Inter-laboratory reproducibility requirements Measured component content

Appendix E

(Informative) Concentration and recovery of MCPA and MCPB in different matrices Table E.1 Concentration and recovery of MCPA and MCPB in different matrices Average recovery (%) MCPA MCPB Add concentration (mg/kg) Add concentration (mg/kg) 0.01 0.05 0.1 0.01 0.05 0.1 Beef 91.5 101.7 93.8 87.5 100 105.2 Pork sausage 107.6 98.2 102.4 77.1 78.9 95.6 Fish 94.8 84.3 82.4 93.3 82.7 82.3 Chicken 94.8 97.0 99.5 90.7 95.5 95.9 Beef canned 91.0 89.6 93.9 95.5 99.9 98.0. ......

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