摘要
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.
出处
《中国卫生检验杂志》
CAS
2008年第12期2522-2524,共3页
Chinese Journal of Health Laboratory Technology
基金
宁波市自然科学基金项目(2007A610072)
关键词
谷类食物
茚满二酮
正交试验
高效液相色谱法
Cereal
Indandione rodenticide
Orthogonal test
High-performance liquid chromatography