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GB 23200.48-2016 English PDF

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GB 23200.48-2016: Food safety national standard -- Determination of residual residues in food by gas chromatography-mass spectrometry
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Basic data

Standard ID GB 23200.48-2016 (GB23200.48-2016)
Description (Translated English) Food safety national standard -- Determination of residual residues in food by gas chromatography-mass spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 13,168
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 1742-2006
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 23200.48-2016: Food safety national standard -- Determination of residual residues in food by gas chromatography-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 residues residual in food by gas chromatography - mass spectrometry ICS SN/T ×××× - ×××× Detection of Residual Amount of Wild Yanyouyan in Import and Export Food method - Gas Chromatography - Mass Spectrometry Determination of difenzoquat residues in foods for import and export - Gas chromatography mass spectrometry method (For approval) 2005 - × × - × × release 2005 - × × - × × implementation People 's Republic of China State Administration of Quality Supervision, Inspection and Quarantine release People 's Republic of China Entry - Exit Inspection and Quarantine Industry Standard GB 23200.48.2016 Instead of SN/T 1742-2006 National standards for food safety Determination of residual residues in wild Gas chromatography - mass spectrometry National food safety standards- Determination of difenzoquat residue in foods Gas chromatography - mass spectrometry 16 12-18 release.2017-06-18 National Health and Family Planning Commission of the People 's Republic of China Ministry of Agriculture of the People 's Republic of China State Administration of Food and Drug Administration release National Standard of the People 's Republic of China GB

Foreword

This standard will replace SN/T 1742-2006 "import and export food in the wild Yan dry residue detection method of gas chromatography tandem mass spectrometry" Compared with SN/T 1742-2006, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - the name of the "import and 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 1742-2006. National standards for food safety Determination of residual residues in food by gas chromatography - mass spectrometry

1 Scope

This standard specifies the method of gas chromatography-mass spectrometry for the determination of wild wilting residues in foodstuffs (see Appendix A). This standard applies to wheat, corn, pork, beef, wild wild dry residue determination, 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 date of the note applies This document. 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 6882 Analytical laboratory water specifications and test methods

3 principle

The samples were extracted with water-acetone and extracted with methylene chloride solution. The samples were purified by gel column chromatography and then treated with Florisil (Florisil) Solid phase column purification, eluent concentration and dissolved volume, the gas chromatographic - mass spectrometer detection, external standard method quantitative.

4 reagents and materials

Unless otherwise specified, the reagents used are analytically pure and the water is in accordance with the primary water specified in GB/T 6882. 4.1 Reagents 4.1.1 Acetone (CH3COCH3, CAS. 67-64-1). Chromatographic Purification. 4.1.2 Dichloromethane (CH2Cl2, CAS. 75-09-2). Chromatographic pure. 4.1.3 Cyclohexane (C6H12, CAS. 110-82-7). Chromatographic purity. 4.1.4 Ethyl acetate (C4H8O2, CAS. 141-78-6). Chromatographic pure. 4.1.5 n-Hexane (C6H14, CAS. 110-54-3). Chromatographic pure. 4.1.6 anhydrous sodium sulfate (Na2SO4, CAS. 15124-09-1). 650 ℃ burning 4 h, stored in a sealed container in reserve. 4.2 solution preparation 4.2.1 sodium sulfate aqueous solution (20 g/L). take 20g anhydrous sodium sulfate, water volume to 1000mL, shake back standby. 4.3 standards 4.3.1 Wild Yandeng Standard Substance. See Appendix A. 4.4 standard solution preparation 4.4.1 wild wild dry standard stock solution. accurately weighed the right amount of wild Yan dry standard material, with acetone prepared into a concentration of 100 g/mL Standard stock solution, the standard reserve solution away from 0 ℃ ~ 4 ℃ preservation, shelf life of 6 months. 4.4.2 wild Yan dry standard working solution. According to the testing requirements, respectively, the above standard reserve solution in the volumetric flask, diluted with acetone To the standard preparation of the appropriate concentration of the standard working solution, the standard working solution away from 0 ℃ ~ 4 ℃ preservation, shelf life of one month. 4.5 Materials 4.5.1 Florisil Solid phase extraction column. 1.0 g, or equivalent.

5 instruments and equipment

5.1 Gas Chromatography-Mass Spectrometer. with quality selection detector. 5.2 Gel chromatograph. with unit pump and fraction collector. 5.3 Analysis of balance. 0.01 g and 0.0001 g. 5.4 Rotary Evaporator. 5.5 anhydrous sodium sulfate column. 7.5 cm × 1.5 cm (id), built-in 5 cm high anhydrous sodium sulfate. 5.6 stoppered conical flask. 250 mL. 5.7 separatory funnel. 250 mL. 5.8 Concentrated bottles. 50 mL, 250 mL. 5.9 Filtration. 0.45 m 5.10 oscillator.

6 Preparation and storage of samples

6.1 Preparation of the sample 6.1.1 Grain The sample was shrunk to 1 kg by quarter, homogenized with an attritor and passed through a 2.0 mm round hole screen. Mix, are divided into two as The sample is packed in a clean vial, sealed and marked. 6.1.2 Meat and meat products A sample of about 1 kg was taken from all the samples taken and crushed evenly through the crusher and divided into two portions Clean the container as a sample. Sealed and marked. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 6.2 Sample storage Grains and oilseeds are stored at 0-4 ° C; meat and meat samples are cryopreserved at -18 ° C or lower. In the sampling and sample operation In the course of the process, the sample should be prevented from being contaminated or the residue content changes.

7 Analysis steps

7.1 Extraction Weigh the sample about 20 g (accurate to 0.1 g) in a 250 mL stoppered flask, add 100 mL of water - acetone (14), shake Extraction for 30 min, the extract was filtered in 250 mL concentrated bottle. Residue and then 50 mL of acetone repeated extraction time, combined filtrate, And concentrated in a water bath at 40 ° C to about 20 mL. The concentrated extract was transferred to a 250 mL separatory funnel, 150 mL of sodium sulfate aqueous solution and 50 mL of dichloromethane were added, shaking 3 Min, and the layers were separated and the dichloromethane phase was collected. The aqueous phase was extracted twice with 2 x 50 mL of methylene chloride and the dichloromethane phases were combined. Dehydrated by anhydrous sodium sulfate column, collected in 250 mL concentrated flask, concentrated in a 40 ° C water bath to near dry, add 5 mL of cyclohexane - Ethyl acetate (1 1) to dissolve the residue and filter with a 0.45 m filter to be purified. 7.2 Purification 7.2.1 Gel Chromatography (GPC) 7.2.1.1 Gel chromatographic conditions A) Purification column. 700 mm × 25 mm, Bio Beads S-X3, or equivalent. B) Mobile phase. cyclohexane-ethyl acetate (1 1). C) Flow rate. 5.0 mL/min. D) Sample dosing ring. 5.0 mL. E) Pre-elution volume. 50 mL. F) Elution volume. 150 mL. G) Collection volume. 75 mL to 10.5 mL. 7.2.1.2 Gel Chromatographic Purification Procedure The 5 mL of the purified liquid was purified under the conditions specified in 7.2.1.1, and the collected fractions in the combined fraction collector were mixed in 50 mL of concentrated In the 40 ° C water bath spin concentrated to near dry, add 2 mL of n-hexane to dissolve the residue, to be purified. 7.2.2 Solid Phase Extraction Purification (SPE) The Florisil solid phase extraction column was pre-eluted with 5 mL of n-hexane and the sample was poured into the column and then treated with 8 mL N-hexane-ethyl acetate (4 1). The whole eluate was collected in a 50 mL concentration flask and concentrated in a 40 ° C water bath dry. Dissolved in acetone and set to 2 mL, gas chromatography - mass spectrometry and confirmed. 7.3 Determination 7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions A) Column. DB-5 MS quartz capillary column, 30 m × 0.25 mm (id), film thickness 0.25 m, or equivalent. B) Column temperature. 50 ° C (for 2 min) 20 ° C/min 180 ° C (for 1 min) 10 ° C/min 270 ° C 10 min). C) Inlet temperature. 280 ° C. D) chromatographic - mass spectrometer interface temperature. 270 ° C. E) Carrier gas. helium, purity ≥99.999%, flow rate 1.2 mL/min. F) Injection volume. 1 μL. G) Injection method. no split injection, 1.5 min after the opening valve. H) ionization mode. EI. I) Ionization energy. 70 eV. J) Measurement method. Select the ion monitoring mode. K) Monitoring ions (m/z). See Appendix A. L) solvent delay. 5 min. 7.3.2 Determination and confirmation of chromatography According to the sample in the wild Yan dry content, selected peak area similar to the standard working solution, the standard working solution and sample solution The response value of the standard working solution and the sample solution should be within the linear range of the instrument detection. Under the same experimental conditions, the mass retention time of the material to be tested in the sample solution was the same as that of the standard working solution and the background The selected ions in the sample mass chromatogram appear after comparison with the abundance of the selected ions and the abundance of the corresponding ions Within the allowable range (see Table 1 for the permissible range), it is determined that there is a corresponding analyte in the sample. In the above chromatographic conditions, wild Yan dry (M/z) abundance ratio is shown in Appendix A. Gas Chromatography - Mass Spectrometry Ion Chromatogram and The spectra are given in Appendix B, B.1 and Appendix C, C.1. Table 1 Maximum allowable error for relative ion abundance using gas chromatography-mass spectrometry Relative 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 processor or the following formula (1) to calculate the amount of residual residues in the sample. Ai · Csi · V X = ------------------------------. (1) Asi · m Where. Xi - the amount of residue in the sample, in milligrams per kilogram (mg/kg); The peak area of wild leaf in the sample solution; V - the final volume of the sample solution in milliliters (mL); The peak area of the wild goose in the Asi- standard working fluid; Csi - concentration in standard working solution, in micrograms per milliliter (g/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) Together with the requirements of Appendix E. 9.2 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) Together with the requirements of Appendix F. 10% limit and recovery rate 10.1 Quantitation limits The limit of quantification of this method was 0.010 mg/kg. 10.2 Recovery rate When the levels were 0.010 mg/kg, 0.050 mg/kg and 0.200 mg/kg, the addition recovery See Appendix D.

Appendix A

(Informative) Wild leafy CAS number, retention time and monitoring ion abundance ratio Table A.1 CASE CASE, retention time and monitoring ion abundance ratio table No. Chinese name English name CAS number Molecular formula Molecular weight retention time Min Monitor the ion abundance ratio 1 Dryer Drying Difenzoquat 43222-48-6 C18H20N2O4S 360.43 15.80 189 (6), 233 (23), 234 (100), 235 (18) Note. "*" mark ions as quantitative ions

Appendix B

(Informative) Gas Chromatography - Mass Spectrometry Ion Chromatography Figure B.1 Gas Chromatography-Mass Spectrometry Ion Chromatogram of Wild Yandeng Substances Min

Appendix C

(Informative) Gas Chromatography - Mass Spectrometry of Wild Figure C.1 Gas Chromatography-Mass Spectrometry for Wild Goap Standard M/z

Appendix D

(Informative) The recovery rate of wild leaves in different matrices Table D.1 Recovery rates of wild leaves in different substrates NO pesticide name Sample matrix Wheat corn pork beef 1 wild Yan dry 89.0% ~ 94.9% 88.0% ~ 88.3% 86.5% ~ 95.0% 92.4% ~ 93.5%

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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