建立了高效液相色谱-串联质谱(HPLC-MS/MS)同时测定蜂王浆中氟胺氰菊酯、三唑醇、蝇毒磷、吡氟乙草灵、多菌灵、乙基硫菌灵和甲基硫菌灵7种高风险农药残留的分析方法.样品在碱性条件下经乙腈提取,无水硫酸钠脱水后,采用HLB固相萃取小柱富集净化.采用Venusil MP C18色谱柱分离,以0.5 mmol/L乙酸铵水溶液(含0.1%(v/v)甲酸)-甲醇(含0.1%(v/v)甲酸)为流动相,梯度洗脱.在电喷雾离子(ESI)源、正离子模式和多反应监测(MRM)模式下采集数据,内标法定量.结果表明,7种高风险农药在5~100 μg/kg范围内线性关系良好,相关系数(r2)为0.9921~0.9996;方法的检出限和定量限分别为0.5~2.0 μg/kg和1.0~5.0 μg/kg.在高、中、低3个添加水平下7种农药的加标回收率为80.5%~101.3%,相对标准偏差(RSD)为3.6%~9.4%.该法操作简单,灵敏度高,准确可靠,能够满足出口蜂王浆农残限量检测的要求.%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.
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