高效液相色谱法测定饲料中辛硫磷残留量

HPLC Determination of Residual Amount of Phoxim in Feed

提出了高效液相色谱法测定饲料中辛硫磷残留量的方法。样品经乙酸乙酯提取,氨基固相萃取小柱净化,所得净化液以反相C18色谱柱为分离柱,以乙腈-水(65+35)混合溶液为流动相,在检测波长280nm处进行测定。辛硫磷的质量浓度与其峰面积在0.10～0.50mg·L-1范围内呈线性关系,方法的检出限(3S/N)为0.10mg·kg-1。加标回收率在80.0%～88.2%之间,测定值的相对标准偏差(n=5)在1.6%～6.5%之间。

HPLC was applied to the determination of residual amount of phoxim in feed. The sample was extracted with ethyl acetate and purified by passing through NH2-solid phase extraction column. Reverse C18 chromatographic column was used as stationary phase, and a mixed solution of acetonitrile and water （65＋35） was used as mobile phase. UV-detection at 280 nm was adopted in the determinatiom Linear relationship between values of peak area and mass concentration of phoxim was obtained in the range of 0.10--0. 50 mg. L^-1, with detection limit of 0. 10 mg. kg^-1. Values of recovery found by standard addition method were in the range of 80. 0%- 88. 2%, and values of RSD＇s （n=5） in the range of 1.6%--6.5%.