分散液液微萃取/液相色谱串联质谱法快速测定蜂蜜中10种杀螨剂  

Determination of acaricides in honey using optimizied dispersive liquid-liquid microextraction combined with high-performance liquid chromatography-tandem mass spectrometry

作　　者：曾银欢 周靓静 吴慧珍[1] 陈志民[2] 徐杰[2] 方丽珍[2] 莫卫民[1] 吴俐勤[2] 

机构地区：[1]浙江工业大学化学工程学院,杭州310014 [2]浙江省农业科学院农产品质量标准研究所,杭州310021

出　　处：《分析试验室》2015年第2期216-221,共6页Chinese Journal of Analysis Laboratory

摘　　要：采用超声辅助-分散液液微萃取技术,建立快速测定蜂蜜中10种杀螨剂（四螨嗪,喹螨醚,吡螨胺,噻螨酮,乙螨唑,蝇毒磷,哒螨灵,克螨特,螺螨酯,唑螨酯）残留的液相色谱-串联质谱分析方法。电喷雾正离子扫描模式检测10种杀螨剂,基质匹配曲线定量。10种杀螨剂在0.10-100μg/L范围内线性良好,四螨嗪、喹螨醚、噻螨酮、乙螨唑、螺螨酯的定量限（S/N=10）为3.0μg/kg;蝇毒磷、哒螨灵、克螨特的定量限为1.5μg/kg;吡螨胺的定量限为2.0μg/kg;唑螨酯的定量限为2.5μg/kg。10种杀螨剂在10,50,100μg/kg加标浓度下,回收率在72%-107%之间,相对标准偏差RSD〈12%。A rapid high-performance liquid chromatography-tandem mass spectrometric（ HPLC-MS / MS） method has been developed for the determination of ten acaricides（ Clofentezine,Fenazaquin,Tebufenpyrad,Hexythiazox,Etoxazole,Coumaphos,Pridaben,Propargite,Spirodiclofen,Fenpyroximate） in honey with ultrasonic-assistant dispersive liquid-liquid microextraction（ DLLME）. The qualitative and quantitative analysis for the analytes were carried out under the multi-reaction monitoring（ MRM） mode with positive mode in matrix-matched standard method.Under the optimal conditions,the calibration curves were linear in the range of 0. 1 - 100 μg / L for 10 acaricides. The limits of quantitation（ LOQs） were 3. 0 μg / kg for clofentezine,fenazaquin,hexythiazox,etoxazole and spirodiclofen,1. 5 μg / kg for coumaphos,pridaben and propargite,2. 0 μg / kg for tebufenpyrad,and 2. 5 μg / kg for fenpyroximate.The blank honey samples were spiked at three concentration levels of 10,50,100 μg / kg,the recoveries ranged from72% to 107% with the relative standard deviations less than 12%

关 键 词：蜂蜜 杀螨剂 分散液液微萃取 高效液相-色谱串联质谱 

分 类 号：O657.63[理学—分析化学]