固相萃取-超高效液相色谱法测定水中速灭威、异丙威、乙霉威及仲丁威  

UHPLC Determination of Metolcarb,Isoprocarb,Baycarb and Diethofencarb in Water with Solid Phase Extraction

作　　者：王晓楠[1] 潘献辉[1] 

机构地区：[1]国家海洋局天津海水淡化与综合利用研究所,天津300192

出　　处：《理化检验（化学分册）》2013年第11期1368-1370,1374,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：2010年中央级公益性科研院所基本科研业务费专项资金项目(K-JBYWF-2010-G17);2013年中央级公益性科研院所基本科研业务费专项资金项目(K-JBYWF-2013-G14);2013年海洋公益性项目(201305039)

摘　　要：提出了水中速灭威、异丙威、乙霉威及仲丁威的固相萃取-超高效液相色谱测定方法。水样（pH调至4～5）经OasisHLB固相萃取小柱净化，甲醇洗脱，所得净化液以30rC的EclipseXDBC18色谱柱为分离柱，以甲醇-水（70＋30）混合液为流动相，用紫外检测器在波长284nm处进行测定。速灭威、异丙威、乙霉威及仲丁威在-定的质量浓度范围内与峰面积呈线性关系，方法检出限（3S／N）在0．049～1．6μg·L-1之间。在3个浓度水平上对方法做回收试验，测得回收率在92．0％～106％之间，相对标准偏差（n=7）在1．29／6～4．9％之间。UHPLC was applied to the determination of metolcarb, isoprocarb, baycarb and diethofencarb in water with solid phase extraction. The water sample （preadjusted to pH 4-5） was purified by passing through Oasis HLB-solid phase extraction column and eluted with methanol. Eclipse XDB C18 chromatographic column was used as stationary phase at column temperature of 30℃, and a mixture of methanol and water （70＋30） was used as mobile phase. UV-detection at 284 nm was adopted in the determination. Linear relationships between values of peak area and mass concentration of the 4 pesticides were kept in definite ranges, with detection limits（3S/N ）in the range of 0. 049--1.6 μg . L-1. Tests for recovery were made at 3 concentration levels, giving values of recovery in the range of 92.0%--106%with RSD＇s （n=7）in the range of 1.2%--4. 9%.

关 键 词：超高效液相色谱法 固相萃取 水样 速灭威 异丙威 乙霉威 仲丁威 

分 类 号：O652.63[理学—分析化学]