HPLC法同时测定羌活药材中甲基托布津和辛硫磷农药的残留  

Simultaneous determination of thiophanate-methyl and phoxim residues in Notopterygium incisum by HPLC

作　　者：周瑞雪 连云岚 郝云芳 冯贞 李民生 张远芳 李倩 崔广青 ZHOU Ruixue;LIAN Yunlan;HAO Yunfang;FENG Zhen;LI Minsheng;ZHANG Yuanfang;LI Qian;CUI Guangqing(Laboratory of Biological Products,Institute of Drug Testing Technology,Shanxi Provincial Inspection and Testing Center,Taiyuan 030001,China;Laboratory of Traditional Chinese Medicine,Institute of Drug Testing Technology,Shanxi Provincial Inspection and Testing Center)

机构地区：[1]山西省检验检测中心药品检验技术研究所生物制品室,太原030001 [2]山西省检验检测中心药品检验技术研究所中药室

出　　处：《山西医科大学学报》2024年第2期228-232,共5页Journal of Shanxi Medical University

基　　金：全国中药特色技术传承人才培训项目(T20234832005);国家药品抽检计划中药饮片专项(食药监药化监[2017]131号)。

摘　　要：目的建立同时测定羌活中甲基托布津和辛硫磷2种农药残留的HPLC法。方法羌活药材样品加NaCl粉末,以0.1%甲酸乙腈为提取溶剂,通过无水硫酸钠粉末净化,所得净化液以反相C_(18)色谱柱为分离柱,以乙腈∶0.1%甲酸(含10 mmol/L甲酸铵)(70∶30)为流动相,流速0.8 mL/min,在检测波长280 nm处测定2种农药残留的量。结果甲基托布津和辛硫磷配制浓度与峰面积在0.02~0.2μg/mL范围内有良好的线性关系,相关系数为0.9986和0.9993,该方法的检测限分别为4 ng/mL和3 ng/mL。甲基托布津的加标回收率为92.14%~112.56%,辛硫磷的加标回收率为87.85%~103.45%。结论该HPLC检测方法的操作简单、准确而快速,重复性和稳定性均良好,可满足羌活药材中甲基托布津和辛硫磷农药残留检测的要求。Objective To establish an HPLC method for the simultaneous determination of the two pesticide residues,thiophanate-methyl and phoxim,in Notopterygium incisum.Methods The Notopterygium incisum sample and NaCl powder were mixed with 0.1%formic acid acetonitrile as the extraction solvent,and purified by anhydrous sodium sulfate powder.Reverse C_(18) chromatographic column was used as a stationary phase,and a mixed solution of acetonitrile∶0.1%formic acid(containing 10 mmol/L ammonium formate)(70∶30)was used as a mobile phase,the flow rate was 0.8 mL/min,and the detection wavelength was 280 nm.The two pesticide residues were detected by HPLC.Results There was an excellent linear relationship between peak area and thiophanate-methyl and phoxim concentration in the range of 0.02-0.2μg/mL,with a correlation coefficient of 0.9986 and 0.9993.The detection limit of this method was 4 ng/mL and 3 ng/mL for thiophanate-methyl and phoxim,respectively.The recovery rate of spiked samples was 92.14%-112.56%for thiophanate methyl,and 87.85%-103.45%for phoxim.Conclusion The established HPLC is simple,accurate and rapid to detect the pesticide residues,with good repeatability and stability,and can be used for the detection of pesticide residues in Notopterygium incisum.

关 键 词：HPLC 羌活 甲基托布津 辛硫磷 农药残留 

分 类 号：R282[医药卫生—中药学]