摘要
为高效液相色谱法测定环境水样中残留的西维因和抗蚜威的含量,应用了液-液色谱联用技术,实现了在线富集、分离和检测。分析中用YWG-C_(18)(10mm×4.6mm,10μm)和YWG- C_(18)(150mm×4.6mm,10μm)依次作为富集柱和分离柱,以体积比45比55混合的甲醇与水的混合溶液作为流动相,其流速为1.0mL·min^(-1)。选定紫外光度检测的波长为228nm,试样溶液在富集柱上的流速为5.0mL·min^(-1)。此外,对渗漏体积等参素也作了试验,分析信号值与两农药的质量浓度在0.04～1.0μg·L^(-1)范围内呈线性关系。测得方法的检出限(S/N=3)为0.008μg·L^(-1)(西维因)和0.014μg·L^(-1)(抗蚜威),回收试验的结果在93%～119%之间。还对日内和日间精密度进行了试验,测定西维因的日内精密度为1.3%～20.0%,日间精密度为2.3%～22.2%,测定抗蚜威的日内精密度为2.0%～10.8%,日间精密度为2.2%～5.8%。
HPLC determination of residual amounts of carbary and pirimicarb in environmental water by applying LC-LC technique for on-line enrichment, separation and detection was proposed. The YWG-C18 column （10 min×4. 6 mm, 10μm） and YWG-C18 column （150 min×4. 6 mm, 10μ） were used as the enrichment column and the analytical column respectively. A mixture of methanol and water （mixed in the ratio of 45＋55） was used as the mobile phase with the flow-rate of 1 mL · min^-1. Wavelength of UV-detection was taken at 228 nm. Flow-rate of sample solution in the pre-enrichment process was 5 mL · min^-1. Seepage volume and amount of seepage were also studied. Linear relationship between values of the analytical signal and concentration of both pesticides was kept in the range Of 0. 04-1.0 μg · L^-1. Detection limit （S/N=3） of carbaryl was found to be 0. 008 μg · L^-1 and of pirimicarb to be 0. 014 μg · L^-1. Values of recovery found were in the range of 93. 0% - 119%. Within-day and between day precision were tested, giving values of within-day RSD＇s in the range of 1.3%--20. 0% （for carbaryl） and of 2. 0%--10. 8% （for pirimicarh）, and values of between-day RSD＇s in the range of 2. 3% to 22. 2% （for carbaryl） and of 2. 2%--5. 8% （for pirimicarb）.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2008年第9期888-891,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
