| 引用本文: | 林永强,林林,刘广桢,徐丽华.QuEChERS-SPE-UHPLC-MS/MS测定瓜蒌中156种农药残留[J].中国现代应用药学,2018,35(1):17-23. |
| LIN Yongqiang,LIN Lin,LIU Guangzhen,XU Lihua.Determination of 156 Pesticide Residues in Trichosanthis Fructus by QuEChERS-SPE-UHPLC-MS/MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2018,35(1):17-23. |
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| 摘要: |
| 目的 以QuEChERS-SPE为前处理方法，UHPLC-MS/MS为检测仪器，建立瓜蒌中156种农药残留的快速筛查检测方法。方法 采用1%冰乙酸乙腈溶液提取样品，以无水硫酸镁（MgSO4）为脱水剂，经MgSO4、丙基乙二胺（PSA）、C18混合净化剂简单净化，再通过SPE小柱（Waters Prime HLB，3 mL，60 mg）进一步净化，Waters Cortecs C18+柱（100 mm×2.1 mm，1.6 μm）分离，采用UHPLC-MS/MS多反应监测（MRM）模式进行定性和定量分析。结果 156种农药在5~200 μg·L-1内线性关系良好（r<0.995），平均回收率范围为74.9%~116.4%，RSD为1.0%~5.6%，方法的检出限为0.02~20 μg·kg-1，定量限为0.06~50 μg·kg-1。结论 该方法简单、准确、灵敏度高，适合于瓜蒌中多农药残留的同时筛查测定。 |
| 关键词: QuEChERS SPE 超高效液相色谱-串联质谱 农药残留 瓜蒌 |
| DOI：10.13748/j.cnki.issn1007-7693.2018.01.004 |
| 分类号:R917 |
| 基金项目:“重大新药创制”国家科技重大专项（2014ZX09304307-002）；山东省中医药科技发展计划项目（2015-160） |
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| Determination of 156 Pesticide Residues in Trichosanthis Fructus by QuEChERS-SPE-UHPLC-MS/MS |
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LIN Yongqiang, LIN Lin, LIU Guangzhen, XU Lihua
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Shandong Province Institute for Food and Drug Control, Jinan 250101, China
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| Abstract: |
| OBJECTIVE To develope a multi-residue analytical method for the determination of 156 kinds of pesticide residues in Trichosanthis Fructus by QuEChERS-SPE-UHPLC-MS/MS. METHODS The samples were extracted with acetonitrile containing 1% acetic acid, dehydrated by MgSO4, simply purified by a mixed cleaning agents of MgSO4, PSA, and C18, and further cleaned by SPE column(Waters Prime HLB, 3 mL, 60 mg), separated on a Waters Cortecs C18+ column (100 mm×2.1 mm, 1.6 μm) and detected by UHPLC-MS/MS with positive and multiple reaction monitoring mode(MRM). RESULTS The results of all the 156 kinds pesticides showed good linearity in the range of 5-200 μg·L-1(r<0.995). The average recoveries ranged from 74.9% to 116.4%, with the relative standard deviations(RSDs) from 1.0% to 5.6%, the limits of detection(LODs) of the method were among 0.02-20 μg·kg-1, and the limits of quantification (LOQs) were among 0.06-50 μg·kg -1. CONCLUSION The method is simple, accurate and sensitive, can be used for the determination of multi type pesticides in Trichosanthis Fructus. |
| Key words: QuEChERS SPE UHPLC-MS/MS pesticide residues Trichosanthis Fructus |
