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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。
Objective To establish a method for the determination of 10 organophosphorus pesticide residues in Chinese herbal medicines in Qinghai Plateau by capillary gas chromatography. Methods The sample was extracted by acetonitrile, dehydrated by anhydrous sodium sulfate, concentrated and purified by CARB / NH2 solid phase extraction column. The volume of acetone was determined by DB-7 capillary column. The FPD detector Qualitative and quantitative. Results Ten organophosphorus pesticides showed good linearity in the range of 0.10-1.0 μg / mL. The detection limit of this method was 0.0 058-0.060 mg / kg. The standard solutions of 10 organophosphorus mixed solutions were 0.5mg / kg, 6 times in parallel. The average recoveries were 67.1% ~ 120.0% with relative standard deviations of 2.9% ~ 5.7%. Conclusion The method has the advantages of high sensitivity, accuracy and good reproducibility. It is suitable for the determination of 10 organophosphorus pesticide residues in grass-roots units in Chinese herbal medicines.