QuEChERS-气相色谱-三重四极杆质谱法测定白花蛇舌草中18种有机磷农药  

Determination of 18Organophosphorus Pesticide Residues in Hedyotis Diffusa by QuEChERS Coupled with Gas Chromatography-Triple Quadrupole Mass Spectrometry

作　　者：孙婷婷[1] 徐彦红[1] 张雪梅[1] 郑绵冬 SUN Tingting;XU Yanhong;ZHANG Xuemei;ZHENG Miandong(Xuzhou College of Industrial Technology,Xuzhou 221140,China)

机构地区：[1]徐州工业职业技术学院,徐州221140

出　　处：《理化检验（化学分册）》2021年第5期463-469,共7页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：江苏省科技厅自然科学基金项目(BK20161166)。

摘　　要：建立了QuEChERS-气相色谱-三重四极杆质谱法(GC-MS/M S)测定白花蛇舌草中18种有机磷农药(OPPs)含量的方法。用乙腈提取样品中的目标化合物,用无水硫酸镁去除水分,用乙二胺-N-丙基硅烷、C 18吸附剂、石墨化炭黑的混合物去除杂质,得到的溶液供GC-MS/M S分析。用Rxi-5Sil MS毛细管气相色谱柱在程序升温条件下分离样品溶液中的目标化合物,用配有电子轰击离子源的质谱在多反应监测模式下检测,采用空白样品溶液配制的混合标准溶液系列制作工作曲线。结果表明:18种OPPs的质量分数在10.0~1000.0μg·kg^(-1)内与其对应的峰面积呈线性关系,检出限(3S/N)为0.6~3.0μg·kg^(-1);对阴性样品进行加标回收试验,所得18种OPPs的回收率为90.3%~99.9%,测定值的相对标准偏差(n=6)为1.0%~3.6%。方法用于实际样品分析,检出了乙拌磷、马拉硫磷、三唑磷和哒螨灵,检出量为0.2~19.4μg·kg^(-1)。A metod of QuEChERS-gas chromatography-triple quadrupole mass spectrometry(GC-MS/M S)for the determination of 18organophosphorus pesticides(O PPs)in Hedyotis diffusa was established.The target compounds in the sample were extracted with acetonitrile,the water was removed with anhydrous magnesium sulfate,and the impurities were removed with a mixture of ethylenediamine-N-propyl silane,C 18 adsorbent,and graphitized carbon black.The solution obtained was used for GC-MS/MS analysis.Rxi-5 Sil MS capillary chromatographic column was used to separate target compounds in sample solution under temperature-programmed condition,MS with electron impact ion source was used for detection in multiple reaction monitoring mode,and a series of mixed standard solutions with blank sample solution as dilution solvent was used to make working curves.The results showed that mass fractions of 18OPPs were linearly related to the corresponding peak areas in the range of 10.0-1000.0μg·kg^(-1),with detection limits(3 S/N)in the range of 0.6-3.0μg·kg^(-1).The spiked recovery test was made on the negative samples,giving recoveries in the range of 90.3%to 99.9%,and RSDs(n=6)o f determined values were ranged from 1.0%to 3.6%.This proposed method was used for the analysis of actual samples,and ethionate,m alathion,triazophos and pyridaben were detected,with detection amount in the range of 0.2-19.4μg·kg^(-1).

关 键 词：QUECHERS 气相色谱-三重四极杆质谱法 有机磷农药 白花蛇舌草 

分 类 号：O657.63[理学—分析化学]