土壤中辛硫磷和高效氯氟氰菊酯残留量的高效液相色谱分析

Analysis of Phoxim and Lambda-cyhalothrin in Soil by High Performance Liquid Chromatography

从土壤中超声提取辛硫磷和高效氯氟氰菊酯,并采用高效液相色谱法检测其残留量.用乙腈-水(体积比4∶1)作为提取剂,对土壤样品进行超声萃取,提取液经弗罗里硅土小柱净化后,采用反相高效液相色谱法进行残留量测定.使用SynergiTMPolar-RP 80?(250 mm×4.6 mm, 4μm)色谱柱,以乙腈-水(体积比80∶20)为流动相,紫外检测波长为225 nm.结果表明:辛硫磷与高效氯氟氰菊酯的萃取率均高于92%.辛硫磷浓度在0.6~5.4μg/mL范围内和峰面积线性关系良好,线性回归方程A=25.108ρ+45.008,r=0.998 9;高效氯氟氰菊酯浓度在0.4~3.6μg/mL范围内与峰面积呈良好线性关系,线性回归方程A=48.835ρ+56.574,r=0.999 0.该方法简单、快速、准确度高、精密度好,能满足土壤中辛硫磷和高效氯氟氰菊酯残留量的检测要求.

A method was developed for the ultrasonic extraction of phoxim and lambda-cyhalothrin from soil and the detection of their residues by high performance liquid chromatography.The soil samples were ultrasonic extraction by acetonitrile-water(4∶1,by vol)as extractant.The extract was purified with Floridian column.The residue was determined by reversed phase high performance liquid chromatography.With Synergi TM Polar-RP 80(250 mm×4.6 mm,4μm)column was used as the fix phase,the mixture of acetonitrile and water(80∶20,by vol)was used as the mobile phase,the UV detector wavelength was 225 nm.Results show that both phoxim and lambda-cyhalothrin exhibit extraction rates exceeding 92%.The concentration and peak area of phoxim exhibit a good linear relationship between 0.6~5.4μg/mL,and the linear regression equation is A=25.108ρ+45.008,r=0.9989.The concentration and peak area of high-efficiency cypermethrin exhibit a good linear relationship between 0.4~3.6μg/mL,and the linear regression equation is A=48.835ρ+56.574,r=0.9990.The method is simple,rapid,of high accuracy and precision,and can meet the requirements for detecting phoxim and lambda-cyhalothrin residues in soil.