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Oasis HLB固相萃取小柱净化,甲醇洗脱,所得净化液以30 ℃的Eclipse XDB C18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284 nm处进行测定。速灭威、异丙威、乙霉威及仲丁威在一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0.049~1.6 μg·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1.2%~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%.