色谱2018，Vol.36Issue(2)：136-142,7.DOI:10.3724/SP.J.1123.2017.10012
高效液相色谱-串联质谱法同时测定蜂王浆中7种高风险农药残留
Simultaneous determination of seven high risk pesticide residues in royal jelly by high performance liquid chromatography-tandem mass spectrometry
李樱红 1周萍 2徐权华 2赵焕 2邵巧云2
作者信息
- 1. 浙江省食品药品检验研究院,浙江杭州310052
- 2. 杭州蜂之语蜂业股份有限公司,浙江桐庐311500
- 折叠
摘要
Abstract
A method was developed for the simultaneous determination of seven high risk pesti-cides in the royal jelly,eg. tau-fluvalinate,triadimenol,coumaphos,haloxyfop,carbendazim, thiophanate-ethyl and thiophanate-methyl by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS). First,the royal jelly samples were extracted with acetoni-trile under alkaline conditions. After dehydration by anhydrous sodium sulfate,the extracts were enriched and purified through solid-phase extraction(SPE)with Oasis HLB cartridges. Finally,the pesticides were detected by HPLC-MS/MS method. The separation was carried out on a Venusil MP C18 column with gradient elution. Methanol(containing 0.1%(v/v)formic acid)and 0.5 mmol/L ammonium acetate aqueous solution(containing 0.1%(v/v)formic acid)were used as the mobile phases. The detection was achieved using electrospray ionization in positive ion(ESI+)mode and multiple reaction monitoring(MRM)mode for data collection. Quantification was carried out using internal standard method. The results showed that the seven high risk pesticides were linear in the range of 5-100 μg/kg. The linear correlation coeffi-cients(r2)were 0.992 1-0.999 6. The limits of detection(LODs)and limits of quantification (LOQs)of the seven high risk pesticides were 0.5-2.0 μg/kg and 1.0-5.0 μg/kg,respectively. The average recoveries at the three spiked levels were 80.5%-101.3%,and the relative stand-ard deviations were 3.6%-9.4%(n=3). This method is simple,effective and sensitive,and is suitable for the determination of the pesticide residues in royal jelly.关键词
高效液相色谱-串联质谱/固相萃取/农药残留/蜂王浆Key words
high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)/solid-phase extraction(SPE)/pesticide residues/royal jelly分类
化学化工引用本文复制引用
李樱红,周萍,徐权华,赵焕,邵巧云..高效液相色谱-串联质谱法同时测定蜂王浆中7种高风险农药残留[J].色谱,2018,36(2):136-142,7.
