高效液相色谱法测定谷类食物中3种茚满二酮类鼠药研究

Study on determination of indandione rodenticides in cereal by high-performance liquid chromatography

目的：建立能同时检测谷类食物中杀鼠酮、敌鼠、氯敌鼠的灵敏、准确的高效液相色谱分析法。方法：在磷酸盐缓冲溶液（pH=5.5）介质中用乙醇＋乙酸乙酯（5＋95）作萃取剂,通过正交试验,优化提取条件,在ZORBAX SB C18柱（250 mm×4.6 mm i.d.,5μm）上以磷酸盐缓冲液（pH=6.3）、乙腈、甲醇组成的流动相进行梯度洗脱分离,紫外检测。结果：杀鼠酮在0.25～50.0 mg/L,敌鼠、氯敌鼠在0.50～100 mg/L均具有良好的线性,其相关系数均大于0.9993;杀鼠酮的检出限为0.1 mg/L,敌鼠和氯敌鼠的检出限均为0.2 mg/L;回收率在80.0%～95.1%;RSD均小于8.0%。结论：该法灵敏度高、操作简便、准确、适用于谷类食物中茚满二酮类鼠药残留的检测。

Objective：To establish a simple,accurate and sensitive method for the simulataneous determination of three indandione rodenticides in cereal by high-performance liquid chromatography（HPLC）.Methods：The extraction condition was optimized by orthogonal test using ethonal and ethyl acetate（5＋95） as solvent in the phosphate buffer（pH 5.5）.The separation of three indandione rodenticides was performed on a ZORBAX SB C18 column（250 mm × 4.6 mm i.d.,5 μm）using phosphate buffer（pH 6.3）,acetonitrile and methanol as mobile phase by gradient elution.It was a better method that the rodenticides were extracted by 5%（v/v） ethanol in ethyl acetate in the existence of phosphate buffer（pH 5.5） at 40℃ three times by ultrasonic,10min/time.The column temperature was controlled at 30℃.The wavelength of UV detector was set at 280 nm.Results：Pindon in the range of 0.25~50 mg/L and diphacinone and chlorophacinone in the range of 0.50~100 mg/L had a good linear relation with a correlation coefficient more than 0.9993.The detection limit was 0.1 mg/L for pindon,0.2 mg/L for diphacinone and chlorophacinone.The recoveries were 80.0%~95.1 % for the three indandione rodenticides and RSD less than 8.0%.Conclusion：This method is sensitive,fast and accurate to determine trace indandione in cereal.