QuEChERS-液相色谱串联质谱法快速检测猕猴桃中的氯吡脲及其代谢产物

Determination of Forchlorfenuron and Its Metabolites in Kiwifruit Using QuEChERS-LC-MS/MS

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。

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.