青海高原主要中药材中有机磷类农药残留的测定

目的建立毛细管气相色谱法测定青海高原中药材中10种有机磷农药残留的分析方法。方法样品经乙腈超声提取,无水硫酸钠脱水,浓缩后经石墨化碳(CARB)/氨基(NH2)串联固相萃取柱提纯净化,丙酮定容,采用DB-7毛细管柱分离,FPD检测器定性定量。结果 10种有机磷农药在0.10～1.0μg/mL的浓度范围内呈较好的线性关系,该方法的最低检出限为0.0 058～0.060mg/kg。10种有机磷混合标准溶液添加量为0.5mg/kg,平行测定6次,平均回收率为67.1%～120.0%,相对标准偏差为2.9%～5.7%。结论该方法具有较高灵敏度、准确、重现性好等优点,适于中药材中10种有机磷类农药残留在基层单位的测定。

Determination of organophosphorus pesticide residues in main Chinese herbal medicines in Qinghai Plateau

Objective To establish a capillary gas chromatography method to determinate the 10 kinds of organophosphorus pesticide residues in Chinese herbal medicines in Qinghai plateau.Method The samples were extracted by acetonitrile ultrasonic,dehydrated by anhydrous sodium sulfate,purified by graphitized carbon(CARB) / amino(NH2) solid-phase extraction column after concentration,determined constant volum by acetone,separated by DB-7 capillary column,and determined the nature and quantification by FPD detector.Results These 10 kinds of organophosphorus pesticides presented better linear relation in a concentration range of 0.10～1.0g/mL.The lowest detection limit of this method was between 0.0058 mg/kg and 0.060 mg/kg.The additive amount of mixed standard solution of these 10 organophosphorus was 0.5mg/kg.It had measured parallelly for 6 times.The average recovery rate was between 67.1% and 120.0%,and the relative standard deviation was between 2.9% and 5.7%.Conclusion This method had high sensitivity,accuracy and repeatability,which was suitable for the measurement of 10 kinds of organophosphorus pesticides residues in Chinese herbal medicine in basic units.