摘要
建立了高效液相色谱-二极管阵列检测水果中涕灭威、西维因、异丙威、仲丁威、马拉硫磷等5种有机磷和氨基甲酸酯农药的方法。前处理方法采用分散固相萃取,样品以乙腈提取,经无水硫酸镁和氯化钠盐析,PSA净化后,进行HPLC-DAD检测。以甲醇/水(体积比70/30)为流动相,流速1 m L/min。DAD检测器的波长设定为210 nm。5种农药在0.04μg/m L^4μg/m L范围内线性相关系数均高于0.99,检出限在0.057μg/m L^0.60μg/m L之间。样品在0.2、0.4、2μg/m L的加标水平时,平均回收率为73.32%~93.12%,RSD为3.46%~9.36%(n=6)。与传统固相萃取方法相比,分散固相萃取具有简便、省时、高精确度和高回收率的优点,可以作为水果中农药残留的日常检测方法。
A method has been developed for five OPPs and Carbamate pesticides （aldicarb,carbaryl, isoprocarb,fenobucarb,malathion） in fruit samples by high performance liquid chromatography coupled with diode array detector （HPLC-DAD）. Dispersive solid-phase extraction （Dis-SPE） has been used for the preparation： the samples extracted with acetonitrile,salted-out by anhydrous magnesium sulfate and sodium chloride, then cleaned up with PSA, finally analyzed by HPLC-DAD. The mobile phase was methanol/water （V/V, 70/30） at a total flow rate of 1 mL/min. The DAD wavelength was 210 nm. The method showed good linearity over the ranges of 0.04μg/mL-4μg/mL for five pesticides with correlation coefficients all above 0.99 , and the limits of detection were 0.057 μg/mL-0.60 μg/mL. The average recoveries ranged from 73.32 % to 93.12 %with the RSD were 3.46 %-9.36 % （n=6） at spiked levels of 0.2, 0.4, 2 μg/mL. Compared with conventional SPE cleanup, dis-SPE greatly simplified and accelerated sample cleanup and less time-consuming. Meanwhile, the high recoveries and good accuracy showed the optimal experimental conditions were satisfied. This method was applied to pesticide residue monitoring in fruits from local markets.
出处
《食品研究与开发》
CAS
北大核心
2015年第12期99-102,共4页
Food Research and Development
关键词
分散固相萃取
HPLC-DAD
有机磷
氨基甲酸酯
dispersive solid-phase extraction （dispersive SPE）
high performance liquid chromatography-diode array detector （HPLC-DAD）
organophosphorus
carbamate pesticides
