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机构地区:[1]陕西师范大学,西安710061 [2]陕西出入境检验检疫局,西安710068
出 处:《化学分析计量》2013年第3期9-13,共5页Chemical Analysis And Meterage
基 金:国家质检公益性科研项目(201010040);国家质检总局科研项目(2009IK285)
摘 要:建立气相色谱-质谱(GC-MS)法测定中药材中81种农药残留的分析方法。样品用含0.1%乙酸的乙腈提取后用GPC或GPC-SPE固相萃取净化,在选择离子监测模式(SIM)下对天麻、杜仲、金银花、山茱萸进行测定。方法在0.01~1.0μg/mL范围内具有良好的线性关系,相关系数均大于0.999,检出限为6.0~31.9μg/kg,加标回收率为60.8%~128.9%,测定结果的相对标准偏差为7.6%~18.9%(n=6)。该方法操作简便,灵敏度、准确度和精密度均符合农药多残留检测技术要求,适用于中药材中81种农药多残留的测定。The determination of 81 pesticide residues in Chinese herbal medicines by gas chromatography-mass spectrometry(GC-MS) was developed. Samples were extracted with 0.1% acetic acid-acetonitrile solution, then cleaned up with GPC or GPC-SPE, and determined by GC-MS with selective ion monitoring(SIM) mode. The result showed that a good linear relationship was obtained in the range of 0.01-1.0 μg/mL. The correlation coefficients were larger than 0.999. The detection limits were 6.0-31.9 μg/kg, the recoveries were 60.8%-128.6% and the relative standard deviations of determination results were 7.6%-18.9%(n=6). The proposed method is highly sensitive, accurate and reliable to meet the requirements of the multiple pesticide residues analysis in Chinese herbal medicines.
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