高效液相色谱法测定小麦籽粒中杀雄嗪酸残留

Determination of Clofencet in Wheat Grain by High Performance Liquid Chromatography

建立了高效液相色谱法(HPLC)切换波长检测小麦籽粒中化学杂交剂SQ-1主成分杀雄嗪酸残留的方法。采用改进的QuEChERS方法进行样品前处理,以80%乙醇作为提取溶剂,以PSA(primary secondary amine,N-丙基乙二胺)作为分散净化剂进行分散固相萃取净化。采用Wondasil C18不锈钢柱,以甲醇-0.1%乙酸水溶液(70∶30,V/V)为流动相,流速:1.0 mL/min,切换检测波长程序:0.01～5.00 min,283 nm;5.01～6.30 min,220 nm;6.31～10.00 min,283 nm。结果表明:杀雄嗪酸在0.40～80.00 mg/L范围内线性关系良好,相关系数r=0.9999,在3个添加水平(1.00,8.00和60.00 mg/kg)范围内,平均加标回收率在82.12%～93.20%之间,相对标准偏差为1.1%～1.9%,检出限为0.020 mg/L。

A method for the determination of clofencet of chemical hybridizing agent SQ-1 in wheat grain has been established by switching detection wavelength in high performance liquid chromatography.Clofencet was extracted with 80% of ethanol and cleaned up by dispersive solid phase extraction using primary secondary amine.Diamonsil C18 column with the mobile phase consisted of methanol-0.1% HOAc（70 ∶ 30,V/V） was used for the chromatographic separation at a flow rate of 1.0 mL/min,switching wavelength program was： 0.01-5.00 min,283 nm;5.01-6.30 min,220 nm;6.31-10.00 min,283 nm.A good linear relationship was obtained in the range of 0.40-80.00 mg/L with the correlation coefficient 0.9999.The average recoveries of clofencet were 82.12%-93.20% and the RSD were 1.1%-1.9%,and the detection limit was 0.020 mg/L.