离子液体[C4 mim][PF6]超声辅助萃取/LC-MS/MS法测定水中痕量溴敌隆及溴鼠灵  

Simultaneous Determination of Bromoadiolone and Brodifacoum in Water by LC-MS /MS and Ultrasonic Assisted Extraction with Ionic Liquid [C_4mim][PF_6]

作　　者：陈晓红[1,2] 魏晓琴[3] 蔡美强[3] 赵永纲[1,2] 潘胜东[1,2] 金米聪[1,2] 

机构地区：[1]宁波市疾病预防控制中心浙江省微量有毒化学物健康风险评估技术研究重点实验室,浙江宁波315010 [2]宁波市疾病预防控制中心宁波市毒物研究与控制重点实验室,浙江宁波315010 [3]浙江工商大学环境科学与工程学院,浙江杭州310035

出　　处：《分析测试学报》2014年第6期648-652,共5页Journal of Instrumental Analysis

基　　金：国家自然科学基金项目(20977083,21377114);浙江省医药卫生平台重点计划项目(2011ZDA024)

摘　　要：建立了离子液体超声辅助萃取/高效液相色谱-串联质谱联用测定水中溴敌隆和溴鼠灵的方法。采用疏水性离子液体1-丁基-3-甲基咪唑六氟磷酸盐[C4mim][PF6]萃取样品,考察了试样体积、pH值、温度、超声萃取时间和无机盐含量等因素对萃取效率的影响。待测物在XDB C18（150 mm×2.1 mm,5μm）色谱柱上,以甲醇-0.2%乙酸（85∶15）为流动相,电喷雾（ESI）电离负离子多反应监测模式（MRM）进行测定。在优化萃取条件下,溴敌隆和溴鼠灵在0.005～1.0μg·L-1范围内具有良好线性,相关系数（r）大于0.999,回收率为91.0%～97.8%,日内相对标准偏差为1.1%～6.6%,日间相对标准偏差为2.5%～9.1%,定量下限为0.005μg·L-1。建立的方法简便、干扰少、特异性强,可用于环境水样中痕量溴敌隆和溴鼠灵的测定。A method was developed for the simultaneous determination of bromoadiolone and brodifacoum in water by liquid chromatography coupled with tandem mass spectrometry（ LC-MS /MS） and ultrasonic assisted extraction with ionic liquid [C4mim][PF6]. An ionic liquid,1-butyl-3-methylimidazolium hexafluorophosphate（ [C4mim][PF6]） was used to extract the rodenticides in water samples. The extraction parameters,including sample volume,temperature,ultrasonic extraction time,inorganic salt concentration and solution pH were investigated. The separation of target compounds was performed on an XDB C18（ 150 mm ×2.1 mm,5 μm） column with methanol-0. 2%acetic acid（ 85 ∶ 15） as mobile phase. The detection was carried out by LC-MS /MS using a negative electrospray ionization interface in multi-reaction monitoring（ MRM） mode. Calibration curves were linear within the range of 0. 005-1. 0 μg·L-1with correlation coefficients more than 0. 999.The limits of quantitation（ LOQs） were both 0. 005 μg·L-1. The extraction recoveries were between91. 0% and 97. 8%,the intra-day RSDs were between 1. 1% and 6. 6%,and the inter-day RSDs were between 2. 5% and 9. 1%. The developed method was simple,accurate and distinctive,andcould be used for the determination of trace bromoadiolone and brodifacoum in environmental water.

关 键 词：超声辅助离子液体分散液相微萃取 水 1-丁基-3-甲基咪唑六氟磷酸盐 溴敌隆 溴鼠灵 液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学] S482.55[理学—化学]