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SN/T 0654-2019 English PDF

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SN/T 0654-2019: (Determination of Clenbuterol Residues in Exported Fruits Gas Chromatography and Gas Chromatography-Mass Spectrometry / Mass Spectrometry)
Status: Valid

SN/T 0654: Evolution and historical versions

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SN/T 0654-2019English259 Add to Cart 3 days [Need to translate] (Determination of Clenbuterol Residues in Exported Fruits Gas Chromatography and Gas Chromatography-Mass Spectrometry / Mass Spectrometry) Valid SN/T 0654-2019
SN 0654-1997English479 Add to Cart 3 days [Need to translate] Method for the determination of captan residues in fruits for export Obsolete SN 0654-1997

PDF similar to SN/T 0654-2019


Standard similar to SN/T 0654-2019

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Basic data

Standard ID SN/T 0654-2019 (SN/T0654-2019)
Description (Translated English) (Determination of Clenbuterol Residues in Exported Fruits Gas Chromatography and Gas Chromatography-Mass Spectrometry / Mass Spectrometry)
Sector / Industry Commodity Inspection Standard (Recommended)
Classification of Chinese Standard C53
Classification of International Standard 67.050
Word Count Estimation 11,145
Date of Issue 2019-12-27
Date of Implementation 2020-07-01
Issuing agency(ies) General Administration of Customs

SN/T 0654-2019: (Determination of Clenbuterol Residues in Exported Fruits Gas Chromatography and Gas 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.
Determination of captan residues in fruits for Export GC and GC-MS/MS method The People's Republic of China Entry-Exit Inspection and Quarantine Industry Standards Replace SN/T 3847-2014, SN/T 2220-2008 Determination of captan residues in export fruits by gas chromatography and gas chromatography-mass spectrometry/mass spectrometry 2019-12-27 release 2020-07-01 Implementation Issued by the General Administration of Customs of the People's Republic of China Replace standard SN 0654-1997

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009. This standard replaces SN 0654-1997 "Test Method for Captan Residues in Exported Fruits". Compared with SN 0654-1997 "Test Method for Captan Residues in Exported Fruits", the main technical changes of this standard are as follows. -The standard name was revised to "Determination of Captan Residues in Exported Fruits by Gas Chromatography and Gas Chromatography-Mass Spectrometry/Mass Spectrometry"; -Added pears, oranges, oranges, peaches, mulberries, grapes, kiwis, strawberries, olives, lychees, mangos, bananas, and fire dragons Substrates such as fruit, watermelon, cantaloupe, etc., delete the sampling link; --Modified the sample preparation method, and changed the solid phase extraction method to the matrix dispersion solid phase extraction method; --Revised the limit of quantification of the method. gas chromatography is 0.02 mg/kg, and gas chromatography-mass spectrometry/mass spectrometry is used as 0.01mg/kg; --Using gas chromatography to replace the high performance liquid chromatography in the original standard; --- Added gas chromatography-mass spectrometry/mass spectrometry as a confirmation method. Please note that some of the contents of this document may involve patents. The issuing agency of this document is not responsible for identifying these patents. This standard was proposed and managed by the General Administration of Customs of the People's Republic of China. Drafting organization of this standard. Zhengzhou Customs of the People's Republic of China. The main drafters of this standard. Zhang Shoujie, Liu Shengnan, Qiao Qing, Hua Xiangmei, Sun Wuyong, Zhu Weixia, Zhang Shuxia, Wang Sufang, Zhang Yujuan, Pang Wenyue, Xin Ying. The previous editions of the standards replaced by this standard are as follows. Determination of Captan Residues in Exported Fruits

1 Scope

This standard specifies the gas chromatography and gas chromatography-mass spectrometry/mass spectrometry methods for the detection of captan residues in exported fruits. This standard applies to apples, pears, oranges, oranges, peaches, mulberries, grapes, kiwis, strawberries, olives, lychees, mangoes, Determination of captan in banana, dragon fruit, watermelon, melon and other fruits.

2 Normative references

The following documents are indispensable for the application of this document. For dated reference documents, only the dated version is applicable to this file. For undated reference documents, the latest version (including all amendments) is applicable to this standard. GB 2763 National Food Safety Standard Maximum Residue Limits of Pesticides in Food GB/T 6682 Analytical laboratory water specifications and test methods

3 Method summary

Captan in the sample is soaked in phosphoric acid solution, extracted with acetonitrile by vortexing, and purified by matrix dispersion solid phase extraction, then injected into the gas phase Chromatography or gas chromatography-mass spectrometry/mass spectrometry is used for determination, and external standard method is used for quantification.

4 Reagents

Unless otherwise specified, all experimental reagents are analytically pure, and the experimental water meets the requirements of first-grade water in GB/T 6682. 4.1 n-hexane. chromatographically pure. 4.2 Acetonitrile. chromatographically pure. 4.3 PSA (primary secondary amine) as filler for bonded silicon solid phase extraction adsorbent. particle size 40μm~70μm. 4.4 Bonded silicon solid phase extraction adsorbent filler octadecyl silane bonded silica gel C18 (ostade-cylsilane). particle size 40μm ~ 70μm. 4.5 Graphitized carbon black filler GCB (graphitized carbon black). the particle size is 40 μm ~ 70 μm. 4.6 Sodium chloride. 4.7 Anhydrous sodium sulfate. Bake in a muffle furnace at 550°C for 4 hours, and at.200°C, take it out and place it in a desiccator for cooling and then bottling for use. 4.8 Phosphoric acid. 4.9 Phosphoric acid solution (10%). Dissolve 10 mL of phosphoric acid (4.8) in water and dilute to 100 mL with water. 4.10 Captan standard (Captan, C9H8Cl3NO2S, CAS NO. 133-06-2). purity ≥ 99%. 4.11 Captan standard stock solution. accurately weigh an appropriate amount of Captan standard and prepare it with n-hexane to make a standard concentration of 0.1 mg/mL. Quasi-stock solution, stored in a brown bottle at 0℃~4℃ in the refrigerator. 4.12 Captan standard working solution. draw an appropriate amount of standard stock solution (4.11) and dilute it with n-hexane into a standard working solution of appropriate concentration. 4.13 Organic phase filter membrane. 0.22 μm.

5 Main instruments and equipment

5.1 Gas chromatograph. with electron capture detector. 5.2 Gas chromatography-mass spectrometer/mass spectrometer. equipped with EI source. 5.3 Balance. Sensitivity is 0.1 mg and 0.01 g. 5.4 Nitrogen blowing instrument. 5.5 Vortex mixer. 5.6 Centrifuge. speed ≥ 5 000 r/min. 5.7 Ultrasonic generator. 5.8 Graduated centrifuge tube. 15 mL.

6 Sample preparation and storage

Take out a representative sample of about 500 g from all the samples taken and treat it in accordance with the requirements of GB 2763.Use a masher to grind and mix all the samples. Evenly, divide them into two parts, put them into clean containers, seal them, mark them, and store them in the freezer below -18°C. In the process of sample preparation and storage, the sample should be prevented from being contaminated or from changing the content of residues.

7 Measurement procedure

7.1 Extraction Weigh 5.0 g sample (accurate to 0.01 g) and place it in a 50 mL centrifuge tube. Add 5 mL 10% phosphoric acid solution (4.9) to soak 5 min, add 25 mL acetonitrile (4.2) and 7 g sodium chloride (4.6) vigorously vortex and shake to extract for 10 min, at 5 000 r/min Centrifuge for 5 min, and take 10 mL of the supernatant in a 15 mL test tube with a stopper for purification. 7.2 Purification Add 100 mg PSA filler, 50 mg C18 filler and 30 mg GCB filler into the above-mentioned stoppered test tube filled with supernatant. Vortex for 1 min, centrifuge at 5,000 r/min for 1 min, and accurately pipette 5 ml of the purification solution into a 15 mL test tube with a stopper, and blow nitrogen to the temperature at 40 ℃ Nearly dry, add 1.0 mL of n-hexane (4.1) to dissolve the residue and sonicate for 15 s, then add 0.1 g of anhydrous sodium sulfate (4.7) to remove water, vortex For 1 min, pass through a 0.22 μm filter membrane and inject it into a gas chromatograph or gas chromatograph-mass spectrometer/mass spectrometer for analysis. 7.3 Determination 7.3.1 Instrument conditions 7.3.1.1 The reference conditions of gas chromatography are as follows. a) Chromatographic column. HP-5, column length 30 m, inner diameter 0.32 mm, film thickness 0.25 μm or equivalent performance column; b) Column temperature program. keep the initial temperature at 50 ℃ for 1 min, increase the temperature to 180 ℃ at 8 ℃/min, keep it for 1 min, and then Increase the temperature to 300 ℃ at 20℃/min and keep it for 2 min; c) Temperature of the inlet. 240℃; d) Detector temperature. 300 ℃; e) Carrier gas. Nitrogen (purity ≥ 99.999%), 1.0 mL/min; f) Makeup gas. nitrogen (purity ≥ 99.999%), 30 mL/min; g) Sampling method. splitless sampling; h) Injection volume. 1.0 μL. 7.3.1.2 The reference conditions of gas chromatography-mass spectrometry/mass spectrometry are as follows. a) Chromatographic column. HP-5 MS, column length 30 m, inner diameter 0.25 mm, film thickness 0.25 μm or equivalent performance column; b) Column temperature program. keep the initial temperature at 50 ℃ for 1 min, raise the temperature to.200 ℃ at 10℃/min, keep it for 1.5 min, and then Increase the temperature to 300 ℃ at 20℃/min and keep it for 2 min; c) Inlet temperature. 260℃; d) Chromatography-mass spectrometry interface temperature. 280℃; e) Ion source temperature. 180℃; f) Carrier gas. helium (purity ≥ 99.999%), 1.0 mL/min; g) Ion source. electron bombardment source (EI source) h) Sampling mode. splitless injection, 1.5 min open valve; i) Injection volume. 1.0 μL; j) Solvent delay. 5 min; k) Scanning mode. Multi-reactive ion monitoring mode (SRM); its parent ion m/z 147.97, product ion m/z are 104.87*, 78.97, 69.93.a 7.3.2 Determination by gas chromatography According to the content of the analyte in the sample solution, select a standard series of working solutions with similar content. To be tested in standard working solution and sample solution The corresponding values of the pesticides should all be within the linear range of the instrument. The standard working solution and the sample solution are of equal volume and inserted into the sample for determination. In the above chromatographic strip The retention time of captan is about 18.81 min. For the chromatogram of the standard product, please refer to Figure A.1 in Appendix A. 7.3.3 Determination and confirmation by gas chromatography-mass spectrometry/mass spectrometry According to the content of the analyte in the sample solution, select a standard working solution with a similar concentration. Captan in standard working solution and sample solution The response value should be within the linear range of the instrument detection. Equal volume of standard working solution and sample solution are inserted into the sample for determination. If the sample solution and the standard In the selected ion chromatogram of the quasi-working solution, there are chromatographic peaks at the same retention time, and the quality of the sample after deducting the background In the chromatogram, the selected ions all appear, and the abundance ratio of the selected ion and the abundance ratio of the corresponding ion of the standard product are within the allowable range. (See Table 1 for the allowable range), then it can be determined that there is a corresponding analyte in the sample. Under the conditions of 7.3.1.2, the retention time of captan is At 18.94 min, the gas chromatography-mass spectrometry/mass spectrometry MRM diagram is shown in Figure A.2.in Appendix A. 7.3.4 Blank test Except that the sample is not weighed, all are carried out according to the above-mentioned measuring conditions and procedures.

8 Calculation and expression of results

Use GC or GC-MS/MS data processing system or formula (1) to calculate the residual amount of captan in the sample. Note. The calculation result needs to be deducted from the blank value.

9 Low limit of determination and recovery rate

9.1 Low limit of determination The lower limit of the determination of this method is 0.02 mg/kg by gas chromatography, and 0.01 mg/kg by gas chromatography-mass spectrometry/mass spectrometry. 9.2 Recovery rate The experimental data of the added concentration and recovery rate of the sample are shown in Table 2 and Table 3.

Appendix A

(Normative appendix) Gas Chromatography and Gas Chromatography-Mass/Mass Spectra of Captan Figure A.1 Gas chromatographic standard spectrum of captan (0.02 mg/L) Figure A.2 MRM diagram of captan standard solution gas chromatography-mass spectrometry/mass spectrometry (0.01 mg/L)

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