GB 23200.84-2016 English PDF

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GB 23200.84-2016: Food safety national standard -- Determination of Methanol -- DDT Residues in Meat by Gas Chromatography -- Mass Spectrometry
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Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
GB 23200.84-2016	259	Add to Cart	3 days	Food safety national standard -- Determination of Methanol -- DDT Residues in Meat by Gas Chromatography -- Mass Spectrometry	Valid

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GB/T 38211   GB/T 18418   GB/T 18419   GB 23200.77   GB 23200.78   GB 23200.76   

Basic data

Standard ID: GB 23200.84-2016 (GB23200.84-2016)
Description (Translated English): Food safety national standard -- Determination of Methanol -- DDT Residues in Meat by Gas Chromatography -- Mass Spectrometry
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Word Count Estimation: 13,142
Date of Issue: 2016-12-18
Date of Implementation: 2017-06-18
Older Standard (superseded by this standard): SN/T 0529-2013
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 23200.84-2016: Food safety national standard -- Determination of Methanol -- DDT Residues in Meat 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 Methanol - DDT Residues in Meat by Gas Chromatography - Mass Spectrometry ICS GB National Standards of People's Republic of China Instead of SN/T 0529-2013 National standards for food safety Determination of Methanol - DDT Residue in Meat Gas chromatography - mass spectrometry National food safety standards- Determination of methoxychlor residue in meat 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 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 0529-2013 "Method for the determination of methotrexate residues in exported meat by gas chromatography/mass spectrometry". Compared with SN/T 0529-2013, the main changes are as follows. - Standard text format is modified to food safety standard text format; - the name and scope of the "export of meat" to "meat"; - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN 0529-1996; -SN/T 0529-2013. National standards for food safety Determination of Methanol - DDT Residues in Meat by Gas Chromatography - Mass Spectrometry

1 Scope

This standard specifies the method of gas chromatography-mass spectrometry for the residual amount of methoxylated DDT in meat. This standard applies to chicken, duck, pork, the determination of residual ozone droplets, other food can refer to the implementation of other food can participate According 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

The samples were extracted with ethyl acetate-cyclohexane (1 1, volume ratio). The extract was concentrated by gel permeation chromatography (GPC) The system was purified and eluted with ethyl acetate-cyclohexane (1 1, by volume). The eluate was concentrated to dryness and constant volume. The gas chromatography-mass spectrometer Ion detection, external standard method.

4 reagents and materials

Unless otherwise stated, all reagents are pesticide residues and water is a Class I water specified in GB/T 6682. 4.1 Reagents 4.1.1 Ethyl acetate (C4H8O2). 4.1.2 Cyclohexane (C6H12). 4.1.3 n-hexane (C6H14). 4.1.4 anhydrous sodium sulfate (Na2SO4). analytical grade, used before the 650 C burning 4 h, stored in a dryer, cooling and standby. 4.2 solution preparation 4.2.1 Ethyl acetate - cyclohexane solution (1 1, volume ratio). take.200 mL of ethyl acetate, add.200 mL of cyclohexane, shake the standby. 4.3 standards 4.3.1 Methoxychloride, C16H15Cl3O2, relative molecular weight. 345.66, CAS. 72-43-5). pure Degrees ≥ 99%. 4.4 standard solution preparation 4.4.1 Methanol DDT standard stock solution. accurately weighed the appropriate amount of methanoxazole standard, with n-hexane prepared into 100 μg/mL Standard storage solution, dark in 0 oC ~ 4 oC preservation, shelf life of 6 months. 4.4.2 Methanol Drops Standard Working Solution. According to the testing requirements, absorb the appropriate amount of the above standard solution in the volumetric flask, Alkaline Dilute the standard working solution with appropriate mass concentration and keep it at 0 oC ~ 4 oC for 1 month.

5 instruments and equipment

5.1 Gas Chromatography - Mass Spectrometer. Equipped with electron impact source (EI). 5.2 Tissue crusher. 5.3 Homogenizer. 5.4 Rotary Evaporator. 5.5 Analytical balance. 0.01 g and 0.0001 g. 5.6 Centrifuge. 5.7 Gel Permeation Chromatography System (GPC). A purification column containing a Biobeads S-X3 filler. 5.8 Scroll Mixer.

6 Sample preparation and storage

6.1 Preparation of the sample Remove some of the representative samples from the original sample, the sampling site according to GB 2763 Appendix A implementation, into the high-speed tissue crusher Broken evenly. Fully mixed, with a four-point split out of not less than 500 g as a sample. Into a clean container, marked with a mark after sealing. 6.2 Sample storage The sample was stored at -18 ° C or lower. During sample preparation and storage operations, the sample should be protected from contamination or changes in residue content.

7 Analysis steps

7.1 Extraction Weigh 10 g (accurate to 0.01 g) sample in a 100 mL stoppered centrifuge tube, add 20 g of anhydrous sodium sulfate, add ethyl acetate- Cyclohexane (1 1, volume ratio) 40 mL, homogeneous 2 min, 4000 r/min centrifugation 5 min, the supernatant through the anhydrous sodium sulfate with a funnel, Collected in 100 mL rotary vials, the residue and then add 20 mL of ethyl acetate - cyclohexane (1 1, volume ratio), according to the above steps to extract a The combined extracts were concentrated to near dryness by rotary evaporation at 40 ° C. 7.2 Purification 7.2.1 Gel Permeation Chromatographic Conditions Gel permeation chromatography conditions are as follows. A) Purification column..200 mm × 25 mm, containing Bio-Beads S-X3 packing; B) mobile phase. ethyl acetate-cyclohexane mixed solvent (1 1, volume ratio); C) Flow rate. 4.7 mL/min; D) Injection volume. 5 mL; E) Start collection time. 9.5 min; F) End of collection time. 13 min. 7.2.2 Gel permeation chromatography purification The residue was dissolved in 10 mL of ethyl acetate-cyclohexane (1 1, by volume) and washed, transferred into a gel permeation chromatography vial, Mix well. If there is a granular substance present, it is centrifuged or filtered. 5 mL of the sample was injected into a calibrated GPC tube and chromatographed by gel permeation System for purification. Eluting with ethyl acetate-cyclohexane solution (1 1, by volume) and the eluate was collected in 100 mL of pear-shaped flask. in 40 ℃ below the rotation of evaporation to near dry. It was dissolved with n-hexane (or other suitable solvent) and fixed to 1.0 mL. 7.3 Determination 7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions A) Column. DB-35MS (30 m × 0.25 mm × 0.25 μm) quartz capillary column or equivalent. B) Column temperature. 80 ℃ for 1 min, then 20 ℃/min program temperature to 180 ℃, keep 3 min, then 20 ℃ / Min program to 230 ℃, keep 7 min, to 10 ℃/min program temperature to 290 ℃, keep 10 min. C) Inlet temperature. 260 ° C. D) Injection method. no split injection. E) Injection volume. 1 μL. F) Carrier gas. helium, purity ≥99.999%, flow rate 1.0 mL/min; G) electron bombardment source. 70 eV; H) ion source temperature. 230 ° C; I) GC-MS interface temperature. 280 ° C; J) Select ion monitoring (SIM). Quantitative ion. 227; Qualitative ion. 344,274. 7.3.2 Qualitative determination Respectively, the same volume into the standard working solution and sample solution in the gas chromatography - mass spectrometer, according to the above conditions for analysis, The peak time was 23.5 min. The chromatogram of the standard is shown in Appendix A, Figures A.1, A.2, A.3. When the sample is measured, if the color is detected The peak retention time is consistent with the retention time of the standard, and the abundance of the selected ions is greater than the abundance of the corresponding ions of the standard In the range permitted by Table 1, it is judged that there is methanoxazole in the sample. Table 1 Maximum allowable error of relative ion abundance using gas chromatography-mass spectrometry 7.3.3 Quantitative determination Quantitative use of a single ion quantitative, the preparation of a series of standard solution concentration, the peak area and the relationship between the concentration of external standard quantitative determination. 7.4 blank experiment Unless the sample is not weighed, according to the above steps.

8 results are calculated and expressed

Use the chromatographic data processor or the formula (1) to calculate the residual content of methoxazole in the sample. MA VcA  (1) Where. X - Residual content of methanoxazole in the sample in milligrams per kilogram (mg/kg); A - the chromatographic peak area of methoxazole in the sample solution; As - the chromatographic peak area of methoxazole in standard working solution; C - mass concentration of methanoxazole in standard working solution in micrograms per milliliter (μg/mL); V - the final volume of the sample solution, in milliliters (mL); M - the final sample of the sample quality, 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 E 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 F requirements. 10% limit and recovery rate 10.1 Quantitation limits The limit of quantification for methotrexate is 0.005 mg/kg. Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10% Allowable relative deviation ± 20% ± 25% ± 30% ± 50% 10.2 Recovery rate When the levels were 0.005 mg/kg, 0.01 mg/kg, 0.02 mg/kg, the recovery rates for methotrexate were given in Appendix D.

Appendix A

(Informative) DNA of DDT pesticide, retention time and monitoring of ion abundance ratio A.1 Methoxy DDT pesticide CAS number, retention time and monitoring ion abundance ratio See Table A.1. Table A.1 CAS Number, Retention Time and Monitoring Ion Abundance Ratio of Methanol DDT Pesticides Pesticide Chinese name Pesticide English name CAS number Molecular formula Molecular retention time Min Monitor the ion abundance ratio

1 Ozone drops

Methoxychlor 72-43-5 C16H15Cl3O2 345.66 23.50 227 (100), 228 (18), 344 (1) Note. "*" mark ions as quantitative ions.

Appendix B

(Informative) DNA - DDT pesticide standard substance total ion chromatogram Figure B.1 Total ion chromatogram of the standard substance for methotrexate

Appendix C

(Informative) Standard Test Method for Methanol - DDT Pesticide Standard Figure C.1 Methanol DDT Pesticide Standard Quality Spectrum Figure C.2 Ozone DDT pesticide standard selection ion mass spectrometry

Appendix D

(Informative) Addition Recovery of Methanol DDT Pesticides in Different Substrates Table D.1 Recovery of Methanol DDT Pesticides in Different Substrates Sample Name Add Concentration/(μg/kg) Recovery% chicken 5 82.8-89.6 10 98.6-104.7 20 100.9-103.2 duck 5 97.4-102.8 10 99.6-103.1 20 101.9-102.7 beef 5 85.2-93.4 10 95.8-97.5 20 93.2-96.2

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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