[关键词]
[摘要]
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400 mg/15 mL,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1~3 μg/L,定量限为5~10 μg/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。
[Key word]
[Abstract]
Forchlorfenuron (1-(2-chloro-4-pyridyl)-3-phenylurea) is a plant growth regulator, which mainly be used to increase the size and weight of kiwifruit. The standards of forchlorfenuron metabolites were obtained by chemosynthesis and forchlorfenuron and its metabolites (4-hydroxyphenyl- forchlorfenuron, 3-hydroxyphenyl-forchlorfenuron, forchlorfenuron-4-O-β-D-glucoside and forchlorfenuron-3-O-β-D- glucoside) in kiwifruit were simultaneously determined by LC-MS/MS with ESI+ under the mode of multiple reaction monitoring (MRM) in this study. The pre-treatment of sample was improved by optimizing PSA addition with acetonitrile as extraction solvent for extraction of clopidourea residue. The results showed that forchlorfenuron and its metabolites had a good linear correlation within a certain concentration range, the relative standard deviations were below 7.1% with a good repeatability, the limit of detection (LOD) was 1~3 μg/L with a limit of quantification (LOQ) of 5~10 μg/L, and recoveris were between 87% and 108% with the PSA addition of 400 mg/15 mL. Therefore, QuEChERS-LC-MS/MS was sensitive and accurate, which could be used for simultaneous determination of forchlorfenuron and its metabolites in kiwifruit.
[中图分类号]
[基金项目]
国家农产品质量安全风险评估项目(GJFP201701403、GJFP201700301、GJFP2016014);陕西省科技统筹创新工程项目(2016KTCQ03-12)