首页|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

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

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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C18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0.02~0.2 μg/mL范围内有良好的线性关系,相关系数为0.998 6和0.999 3,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.
Simultaneous determination of thiophanate-methyl and phoxim residues in Notopterygium incisum by HPLC
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 C18 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 pes-ticide 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 0.02-0.2 μg/mL,with a correlation coefficient of 0.998 6 and 0.999 3.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.

HPLCNotopterygium incisumthiophanate-methylphoximpesticide residues

周瑞雪、连云岚、郝云芳、冯贞、李民生、张远芳、李倩、崔广青

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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

山西省检验检测中心药品检验技术研究所中药室

HPLC 羌活 甲基托布津 辛硫磷 农药残留

全国中药特色技术传承人才培训项目国家药品抽检计划中药饮片专项

T20234832005食药监药化监[2017]131号

2024

山西医科大学学报
山西医科大学

山西医科大学学报

CSTPCD
影响因子:0.931
ISSN:1007-6611
年,卷(期):2024.55(2)
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