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氯吡脲是一种猕猴桃生长过程中常用的植物生长调剂,主要作用是增加猕猴桃果实的尺寸和重量。本研究通过化学合成得到氯吡脲代谢产物标准品,利用高效液相色谱串联质谱(LC-MS/MS)建立了猕猴桃中氯吡脲及其4种代谢产物(4-羟基-氯吡脲、3-羟基-氯吡脲、氯吡脲-4-O-β-D-基葡萄糖苷和氯吡脲-3-O-β-D-基葡萄糖苷)同时检测的定性定量方法。样品前处理利用乙腈作为萃取溶剂提取氯吡脲残留,通过PSA添加量的优化改进了QuEChERS样品前处理方法,5种化合物在LC-MS/MS正离子多反应监测模式下进行质谱分析。结果显示:样品前处理过程中PSA的添加量为400mg/15mL,氯吡脲及其4种代谢产物在一定浓度范围内线性关系良好(r2≥0.995),相对标准偏差(RSD)低于7.1%,重复性好,检出限为1~3μg/L,定量限为5~10μg/L,平均添加回收率87%~108%。该方法快速、准确、灵敏及稳定,能满足果蔬中氯吡脲及其代谢产物残留的同时检测。
Chlorpyrifos is a plant growth regulator commonly used in the growth of kiwifruit, the main role is to increase the size and weight of kiwi fruit. In this study, chlorpyrazide metabolite standard was obtained by chemical synthesis. Chloramphenicol and its four metabolites (4-hydroxy-clopidogrel, 3-hydroxy-clopidogrel, clopidol-4-O-β-D-glucoside and clopidamide -3-O-β-D-glucoside). Sample pretreatment The residue of clopidamide was extracted by using acetonitrile as the extraction solvent. The QuEChERS sample pretreatment method was improved by the optimization of the amount of PSA added. The five compounds were analyzed by LC-MS / MS with multiple reaction monitoring mode. The results showed that the amount of PSA was 400mg / 15mL during the pretreatment of the sample, and the linear relationship was good (r2≥0.995) and the relative standard deviation (RSD) were less than 7.1% , The repeatability is good, the detection limit is 1 ~ 3μg / L, the limit of quantification is 5 ~ 10μg / L, the average recovery is 87% ~ 108%. The method is rapid, accurate, sensitive and stable and can meet the simultaneous detection of clopidamide and its metabolite residues in fruits and vegetables.