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GB/T 20744-2006 PDF EnglishUS$90.00 · In stock · Download in 9 seconds
GB/T 20744-2006: Method for the determination of metronidazole, ronidazole and dimetridazole residues in honey - LC-MS-MS method Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid
Excerpted PDFsFull copy of true-PDF will be delivered in 9 seconds upon purchase: GB/T 20744-2006Similar standardsGB/T 21311 GB/T 21315 GB/T 20756 GB/T 45556GB/T 20744-2006: Method for the determination of metronidazole, ronidazole and dimetridazole residues in honey - LC-MS-MS method---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT20744-2006 GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 67.050 X 04 Method for the determination of metronidazole, ronidazole and dimetridazole residues in honey – LC-MS-MS method Issued on: DECEMBER 31, 2006 Implemented on: MARCH 01, 2007 Issued by. General Administration of Quality Supervision, Inspection and Quarantine; Standardization Administration of PRC. Table of ContentsForeword ... 3 1 Scope ... 4 2 Normative references ... 4 3 Principle ... 4 4 Reagents and materials ... 5 5 Instruments... 6 6 Sample preparation and preservation ... 6 7 Measurement step ... 7 8 Results calculation ... 9 9 Precision ... 9 Appendix A (Informative) Standard substance total ion chromatogram ... 11 Appendix B (Informative) Recovery ... 12ForewordThe Appendix A and Appendix B of this Standard are informative. This Standard was proposed by Qinhuangdao Entry - Exit Inspection and Quarantine Bureau of the People's Republic of China. This Standard shall be under the jurisdiction of the General Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China. Drafting organizations of this Standard. Qinhuangdao Entry - Exit Inspection and Quarantine Bureau of the People's Republic of China, Shandong Agricultural University. The main drafters of this Standard. Pang Guofang, Liu Yongming, Cao Yanzhong, Fan Chunlin, Zhang Jinjie, Li Xuemin, Wu Yanping, Li Jin, Lian Yujing, Lin Zhong. This Standard is the first-time issued national standard. 6.2 Sample preservation PRESERVE the sample under room temperature.7 Measurement step7.1 Extraction WEIGH 10g of sample (accurate to 0.01g); PLACE it in a 50mL plugged glass centrifuge tube; ADD 10 mL of water; MIX it uniformly on the liquid mixer; ADD 20mL of ethyl acetate; USE oscillator to vibrate it for 20min; MAKE it subject to 3000 r/min centrifugation for 5 min; TAKE the supernatant, MAKE it pass through a cylindrical funnel containing 25 g of anhydrous sodium sulfate AND reach into pear-shaped flask. USE 20 mL of ethyl acetate to extract it again, MAKE it pass through the anhydrous sodium cylindrical funnel AND COMBINE with the supernatant; USE a rotary evaporator to evaporate it at 45°C water bath under reduced pressure to about 2mL; PREPARE for purification. 7.2 Purification TRANSFER the aforementioned concentrate into the Carboxylic Acid solid- phase extraction column; respectively USE 4 mL of ethyl acetate and 4mL of acetonitrile to wash pear-shaped flask and extraction column; DISCARD all of the effluent. Under the 65kPa negative pressure, REDUCE pressure and EMPTY the extraction column for 2 min; USE 2 mL of eluent to conduct elution at the flow rate ≤ 3 mL/min; COLLECT the elution solution into a 5mL scale sample tube; USE eluent to make the volume reach to 2 mL; MAKE it pass through 0.20μm filter membrane; PREPARE for the measurement by liquid chromatography - tandem mass spectrometer. 7.3 Measurement 7.3.1 Liquid chromatography conditions a) Chromatography column. Atlantis dC18, 3μm, 150 mm X 2.1 mm (inner diameter) or the equivalent; b) Mobile phase. acetonitrile + 0.1% formic acid solution (30 + 70); c) Flow rate. 200μL/min; d) Column temperature. 30°C; e) Sample injection volume. 20μL. 7.3.2 MS conditionsAppendix B(Informative) Recovery As for the adding concentration and average recovery of the metronidazole, ronidazole, and dimetridazole in this method, see Table B.1. Table B.1 Test data of metronidazole, ronidazole, and dimetridazole adding concentration and average recovery Drug name Adding concentration/(μg/kg) Mean recovery /(%) Metronidazole 0.05 76.0 0.10 79.0 0.20 77.0 1.00 82.4 Ronidazole 0.10 69.5 0.20 78.5 0.40 73.9 2.00 71.7 Dimetridazole 0.10 75.6 0.20 74.9 0.40 75.4 2.00 81.7 ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. |