高效液相色谱法对环境样品中甲基托布津与甲霜灵残留的测定

Residual Determination of Thiophanate-methyl and Metalaxyl in Environment by High Performance Liquid Chromatography

建立了自动固相萃取／高效液相色谱法测定地表水和土壤中甲基托布津和甲霜灵残留的方法。地表水采用C18固相萃取小柱进行富集、净化及浓缩；土壤采用丙酮-二氯甲烷（体积比3：7）溶液振荡萃取，弗罗里硅土小柱净化和浓缩；以乙腈和水为流动相，于230nm波长处对样品进行高效液相色谱检测。甲基托布津和甲霜灵在水中的检出限分别为0．36、3．49μg/L，在土壤中的检出限分别为0．03、0．18mg／kg；在优化实验条件下，甲基托布津和甲霜灵在水样和土壤样品中的添加回收率为77％～105％，精密度为1．2％～8．5％。方法可用于环境样品中甲霜灵和甲基托布津残留量的测定。

A method for determination of thiophanate-methyl（ TM ） and metalaxyl （MEL） in surface water and soil have been developed by automatic solid-phase extraction（SPE） coupled with high performance liquid chromatography（HPLC）. Water sample was cleaned up and concentrated by C18 cartridge, soil sample was firstly extracted by actone -dichloromethane （3 ： 7, by volume）, then purified and concentrated by florisil solid-phase extraction cartridge. The detection of TM and MEL was performed by HPLC using acetonitrile - water as mobile phase and selecting 230 nm as detection wavelength. Under the optimal conditions, the calibration curves showed good linearity on certain concentration of TM and MEL with correlation coefficients not less than 0. 999 5. The detection limits of TM and MEL were 0. 36 μg/L and 3.49 μg/L in water, 0. 03 mg/kg and 0. 18 mg/kg in soil, respectively. Recoveries at three spiked concentration levels ranged from 77% to 105%. The relative standard deviations（RSDs） for real sample spiked with mixed standard were in the range of 1.2% to 8.5%. The SPE/HPLC method could be used to detect MEL and TM in environmental field.