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GB 23200.47-2016 English PDF

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GB 23200.47-2016: Food safety national standard -- Determination of tetramine residues in food by gas chromatography-mass spectrometry
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GB 23200.47-2016English259 Add to Cart 3 days [Need to translate] Food safety national standard -- Determination of tetramine residues in food by gas chromatography-mass spectrometry Valid GB 23200.47-2016

PDF similar to GB 23200.47-2016


Standard similar to GB 23200.47-2016

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Basic data

Standard ID GB 23200.47-2016 (GB23200.47-2016)
Description (Translated English) Food safety national standard -- Determination of tetramine residues in food by gas chromatography-mass spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 13,193
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 1740-2006
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 23200.47-2016: Food safety national standard -- Determination of tetramine 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 tetramine residues in food by gas chromatography - mass spectrometry ICS Instead of SN/T 1740-2006 National standards for food safety Determination of tetramine residues in food Gas chromatography - mass spectrometry National food safety standards- Determination of clofentezine residue in foods Gas chromatography-mass spectrometry 2016-12-18 release 2017-06-18 Implementation 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 Standards of People's Republic of China GB

Foreword

This standard will replace SN/T 1740-2006 "in the import and export of four mites in the detection method of gas chromatography tandem mass spectrometry" Compared with SN/T 1740-2006, 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 1740-2006. National standards for food safety Determination of tetramine residues in food by gas chromatography - mass spectrometry

1 Scope

This standard specifies the method of gas chromatography-mass spectrometry for the presence of tetrandrine residues in food (see Appendix A). This standard applies to the citrus, apple, spinach, broccoli, bovine liver, chicken kidney quadr in the determination of residues, other food can participate According to the implementation of 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 (1 4), washed with methylene chloride solution, and purified by gel column. (Florisil) solid phase column purification, elution concentration and dissolved volume, the gas chromatography - 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 Tetracycline reference substance. see Appendix A. 4.4 standard solution preparation 4.4.1 Tetracycine standard stock solution. accurately weighed the appropriate amount of tetramine 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 Tetracycine 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 Fruits or vegetables Take 500 g of fruit or vegetable sample (not water wash), and then cut the sample into a slurry with a food masher. Mix, are divided into two as a sample, into the clean Sheng Sheng bag, sealed and marked. 6.1.2 Meat and meat products Remove a representative sample of about 1 kg, crushed by the mashed evenly, are divided into two, respectively, into the clean container as a test kind. Sealed and marked. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 6.2 Sample storage The sample was stored at -18 ° C or lower. During sampling and sample preparation, the sample should be protected from contamination or residue The amount of change.

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) The residue was dissolved and filtered 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) Gel 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. 95 mL - 135 mL. 7.2.1.2 Gel Chromatographic Purification Procedure The purified solution of 5 mL was purified under the conditions specified in 6.2.1.1 and the collected fractions in the fraction collector were mixed in 50 mL of concentrated , Concentrated in a 40 ° C water bath to close to dry, add 2 mL of n-hexane - ethyl acetate (4 1) 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) 30 ° C/min 180 ° C (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 content of tetracycine in the sample solution, the standard working solution with similar peak area is selected, and the standard working solution and the sample solution The response value of tetramidazine in standard working solution and sample solution should be within the linear range of 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. Under the above chromatographic conditions, tetracycline (M/z) abundance ratio is shown in Appendix A. Determination of tetramine standard by gas chromatography - mass spectrometry ion chromatography 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 ± 10% ± 15% ± 20% ± 50% 7.4 blank test In addition to the sample, according to the above determination steps.

8 results are calculated and expressed

The residual amount of tetracycline in the sample was calculated using a chromatographic data processor or by the following formula (1). Ai · Csi · V X = ------------------------------. (1) Asi · m Where. Xi - the amount of tetracycine in the sample, in milligrams per kilogram (mg/kg); The peak area of tetracycline in sample solution; V - the final volume of the sample solution in milliliters (mL); The peak area of tetracycine in Asi- standard working fluid; Csi - Concentration of tetracycine in standard working fluid 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 tetracycline is 0.010 mg/kg. 10.2 Recovery rate When the addition level was 0.010mg/kg, 0.050mg/kg, 0.200mg/kg, the addition of tetrathione in different substrates was See Appendix D.

Appendix A

(Informative) The name of the tetramidazine, the retention time and the monitoring of the ion abundance ratio Table A.1 CAS Number, retention time and monitoring ion abundance ratio of tetracycline No. Chinese name English name CAS number Molecular formula Molecular weight retention time Min Monitor the ion abundance ratio 1 tetramidazine Clofentezine 74115-24-5 C14H8Cl2N4 303.15 16.10 102 (82), 138 (100) 304 * (98), 306 (60) Note. "*" mark ions as quantitative ions

Appendix B

(Informative) Gas Chromatography - Mass Spectrometry Ion Chromatography Figure B.1 Chromosomal Chromatography-Mass Spectrometry Ion Chromatogram of Tetracycline Reference Substance Min

Appendix C

(Informative) Gas Chromatography - Mass Spectrometry of Tetrahamidazine Standard Figure C.1 Gas Chromatography-Mass Spectrometry for Tetramine Standards M/z

Appendix D

(Informative) The recovery of tetracycine in different matrices Table D.1 Recovery of tetramidazine in different matrices NO pesticide name Sample matrix Citrus apple spinach broccoli liver chicken kidney 1 tetramidazine 83.8-91.2% 87.0-91.6% 80.8-94.8% 90.5-91.2% 83.8 ~ 95.0 87.5-97.2%

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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