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采用超高效液相色谱-串联质谱法测定白菜和土壤中氰氟虫腙及其主要代谢物残留。

Determination of cyantraniliprole and its major metabolite residues in pakchoi and soil using ultra-performance liquid chromatography-tandem mass spectrometry.

机构信息

Institute for the Control of Agrochemicals, Ministry of Agriculture, Beijing 10026, People's Republic of China.

出版信息

Bull Environ Contam Toxicol. 2012 Oct;89(4):845-52. doi: 10.1007/s00128-012-0752-2. Epub 2012 Aug 30.

DOI:10.1007/s00128-012-0752-2
PMID:22933172
Abstract

A rapid, simple and reliable analytical method was developed for the determination of cyantraniliprole and its major metabolite J9Z38 in pakchoi and soil by using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The sample preparation approach is known as QuEChERS, which stands for quick, easy, cheap, effective, rugged and safe. Samples were extracted with acetonitrile, and cleaned up with dispersive primary and secondary amine sorbent before analysis by UPLC-MS/MS. The limit of quantitation for cyantraniliprole and J9Z38 was 0.01 mg/kg in both pakchoi and soil. Average recoveries of cyantraniliprole and J9Z38 at three fortified levels (0.01, 0.05, 0.1 mg/kg) ranged from 77.8% to 102.5% with relative standard deviation of 1.6%-8.9%. This method has been applied to the analysis of cyantraniliprole and J9Z38 residues in real pakchoi and soil samples selected from field. The results of the residue dynamic experiment showed that the half-life of cyantraniliprole ranged from 2.9 to 6.4 days in pakchoi and 8.7 to 18.2 days in soil, respectively. The final residual levels of cyantraniliprole in pakchoi and soil from Guangdong and Shanghai were below 0.20 and 0.10 mg/kg, respectively; similarly, the final residual levels of J9Z38 in pakchoi and soil from Guangdong and Shanghai were <0.07 and 0.01 mg/kg. These results will be helpful in setting maximum residue limit guidance for cyantraniliprole in pakchoi in China.

摘要

建立了一种超高效液相色谱-串联质谱法(UPLC-MS/MS)用于同时检测小白菜和土壤中虫螨腈及其主要代谢物 J9Z38 的分析方法。样品前处理方法为 QuEChERS,代表快速、简便、廉价、有效、耐用和安全。样品用乙腈提取,用分散型的初级和次级胺吸附剂净化后,采用 UPLC-MS/MS 分析。虫螨腈和 J9Z38 在小白菜和土壤中的定量限均为 0.01mg/kg。在三个添加水平(0.01、0.05、0.1mg/kg)下,虫螨腈和 J9Z38 的平均回收率为 77.8%~102.5%,相对标准偏差为 1.6%~8.9%。该方法已应用于田间采集的实际小白菜和土壤样品中虫螨腈和 J9Z38 残留的分析。残留动态试验结果表明,虫螨腈在小白菜和土壤中的半衰期分别为 2.9~6.4 天和 8.7~18.2 天。广东和上海小白菜和土壤中虫螨腈的最终残留量分别低于 0.20 和 0.10mg/kg,同样,广东和上海小白菜和土壤中 J9Z38 的最终残留量均<0.07 和 0.01mg/kg。这些结果将有助于在中国制定小白菜中虫螨腈的最大残留限量指导值。

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