HPLC-MS/MS测定蜂花粉中4种有机磷类除草剂  

Determination of 4 Organophosphorous Herbicides in Bee Pollen by High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：郭爱静[1] 花中霞[1] 张弘[1] 张世勇[1] 王小青[1] 王可[1] GUO Aijing;HUA Zhongxia;ZHANG Hong;ZHANG Shiyong;WANG Xiaoqing;WANG Ke(Shijiazhuang Technology Innovation Center for Chemical Poison Detection and Risk Early Warning,Shijiazhuang Center for Disease Control and Prevention,Shijiazhuang 050011)

机构地区：[1]石家庄市疾病预防控制中心石家庄市化学毒物检测及风险预警技术创新中心,石家庄050011

出　　处：《食品工业》2021年第4期449-453,共5页The Food Industry

基　　金：石家庄市科学技术研究与发展指导计划(191460733);河北省医学适用技术跟踪项目(GZ2020042)。

摘　　要：首次建立高效液相色谱-串联质谱同时检测蜂花粉中4种有机磷类除草剂(莎稗磷、甲基胺草磷、抑草磷和哌草磷)的分析方法。试样经乙酸乙酯提取、N-丙基乙二胺(PSA)净化、ZORBAX XDB-C18色谱柱(4.6mm×50 mm, 1.8μm)分离,以甲醇/乙腈(50∶50, V/V)和0.1%甲酸水溶液为流动相进行等度洗脱。以电喷雾离子源正离子模式(ESI+)扫描,多反应监测模式(MRM)进行检测。4种有机磷类除草剂的基质匹配标准曲线在1.0~200.0 ng/mL范围内线性关系良好,相关系数(r2)>0.999。空白样品在3个加标水平(5, 20和50μg/kg)下平均回收率为72.2%~89.1%,相对标准偏差(δRSD, n=5)为2.0%~8.9%。方法检出限(LOD, S/N=3)为0.02~0.05μg/kg,定量限(LOQ, S/N=10)为0.07~0.16μg/kg。该方法准确快速、灵敏度高、选择性好,适用于蜂花粉中4种有机磷类除草剂的检测。A method was first developed for the simultaneous determination of 4 organophosphorous herbicides(anilofos, amiprofos-methyl, butamifos and piperophos) in bee pollen by high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS). The samples were extracted by ethyl acetate, and then purified with N-propyl ethylenediamine(PSA). The target compounds were separated on a ZORBAX XDB-C18 column(4.6 mm×50 mm, 1.8 μm). The mixture of methanol/acetonitrile(50∶50, V/V) and 0.1% formic acid solution were used as mobile phase in isocratic elution. The detection was determined, based on positive ion mode of electrospray ionization(ESI+) and multiple reaction monitoring(MRM) mode. The matrix matching calibration curves of 4 organophosphorous herbicides were linear in the range of 1.0-200.0 ng/mL with good correlation coefficients larger than 0.999. The average recoveries at three spiked levels of 5, 20 and 50 μg/kg ranged from 72.2% to 89.1% with the relative standard deviations(δRSD, n=5) of 2.0%-8.9% in the blank sample. The limits of detection and quantitation of the method were 0.02-0.05 μg/kg and 0.07-0.16 μg/kg, respectively. The method was accurate, quick, sensitive and selective, which could be applied in the determination of 4 organophosphorous herbicides in bee pollen.

关 键 词：高效液相色谱-串联质谱(HPLC-MS/MS) 蜂花粉 有机磷类除草剂 检测 

分 类 号：O657.63[理学—分析化学] S896.4[理学—化学]