高效液相色谱柱后衍生法测定谷物中3种氨基甲酸酯类农药残留  

Determination of residues of three carbamate pesticides in grain by high performance liquid chromatography with post-column derivatization

作　　者：赵越超 石家源 杨会宁 张月 徐振斌[1] Zhao Yuechao;Shi Jiayuan;Yang Huining;Zhang Yue;Xu Zhengbin(Jilin Province Grain and Oil Health Inspection and Monitoring Station,Changchun,Jilin 130033)

机构地区：[1]吉林省粮油卫生检验监测站,吉林长春130033

出　　处：《粮食科技与经济》2023年第2期85-88,共4页Food Science And Technology And Economy

摘　　要：采用高效液相色谱柱后衍生法,即将谷物样品粉碎后,经乙腈提取、氮吹、甲醇复溶、固相萃取柱净化、甲醇-二氯甲烷溶液洗脱、氮吹、甲醇定容后,经带有柱后衍生系统和荧光检测器的高效液相色谱仪检测,对谷物中灭多威、涕灭威、克百威3种氨基甲酸酯类农药的残留量进行测定外标法定量。该方法的灭多威、涕灭威、克百威检出限均为0.008 mg/kg;相对标准偏差(RSD)均小于7.5%,加标回收率为80.6%~109.0%,3种农药混合标准曲线最佳线性范围0.01~2.0μg/mL,线性相关系数(R)均大于0.9995。结果表明,该方法具有良好的线性关系,准确性和精密度高,操作简单,适用于谷物中涕灭威、灭多威、克百威农药残留量的同时检测。In this paper,high performance liquid chromatography(HPLC)post-column derivatization method was adopted.After grain samples were crushed,the samples were purified by acetonitrile extraction,nitrogen blowing,methanol redissolution,solid phase extraction column purification,methanol-dichloromethane elution,nitrogen blowing,methanol constant volume,and detected by HPLC with post-column derivatization system and fluorescence detector.Three carbamate pesticide residues of aldicarb,methomyl,and carbofuran in grain were determined and quantified by external standard method.The detection limits of aldicarb,methomyl,and carbofuran were all 0.008 mg/kg.The relative standard deviations(RSD)were all less than 7.5%,and the recoveries ranged from 80.6%to 109.0%.The optimal linear range of the mixed standard curves of the three pesticides was 0.01μg/mL to 2.0μg/mL,and the linear correlation coefficients(R)were all greater than 0.9995.The results showed that the method had a good linear relationship,high accuracy and precision,and was simple to operate.It was suitable for simultaneous determination of aldicarb,methomyl,and carbofuran residues in grain.

关 键 词：固相萃取柱 高效液相色谱柱后衍生法 涕灭威 灭多威 克百威 残留量 

分 类 号：TS210.7[轻工技术与工程—粮食、油脂及植物蛋白工程]