中药中8种有机磷农药残留的检测方法研究-中国方剂学杂志.DOCVIP

中药中8种有机磷农药残留的检测方法研究 邱绿琴1 吴宗彬1 徐小作2 尹江伟2 李行方2 1宝安区中医院药剂科，深圳市518133 ；2 宝安区疾病预防控制中心，深圳市518101 [摘要] 目的：建立了中药中同时测定8种有机磷农药残留（敌敌畏、甲胺磷、乙酰甲胺磷、甲拌磷、乐果、甲基对硫磷、马拉硫磷、对硫磷）的分析方法。方法：采用乙腈提取，经蒸发浓缩，使用配置了双柱（DB-17/HP-1）的气相色谱进行定性定量分析，使用GC-MS法进行确证。结果：8种有机磷在DB-17、DB-1可完全分离；工作曲线在0.5～2.0μmg/mL，相关系数0.9970～0.9999；检出限0.007~ 0.126mg/kg；加标回收实验（n=5）显示，添加水平为0.050.5mg/kg时，平均回收率81.1～113.7%，RSD 2.4～14.1%；添加水平为0.505.0 mg/kg时，平均回收率86.8～116.0%，RSD 4.5～11.7%。结论：本方法灵敏度、准确度和精密度较好，可以做国家标准依据。 [关键词] 农药残留，有机磷农药，中药，气相色谱法 Monitor Method Research of 8 Kinds of Organ-phosphorus Pesticide Residues in Chinese Herbs Qiu Lu-qin1 Wu Zong-bin1 Xu Xiao-zuo2 Yin Jiang-wei 2 Li Xing-fang2 1 Bao`an Hospital Of Traditional Chinese Medical 2 Baoan District Center for Disease Control and Prevention，Shenzhen city， China（518101） [Abstract] Objective：To establish monitor method for 8 kinds of organ-phosphorus pesticide residues in Chinese herbs. Methods：The samples were withdrawn by acetonitrile. then evaporated and concentrated. HP-17/HP-1 double columns gas chromatograph was used for qualitative and quantitative analysis and gas chromatograph-mass spectrometer was used for verify. Results：8 kinds of organ-phosphorus can be separated completely. The correlation coefficient was 0.9970～0.9999 when working Curve was 0.5～2.0μg/mL .The minimum determination limited range is 0.007~ 0.126mg/kg. Recover test(n=5) shows that the average recover rate were 81.1～113.7%，RSD were 2.4～14.1% when add level 0.05mg/kg of organ-phosphorus; the average recover rate were 86.8～116.0%，RSD were 4.5～11.7% when add level 0.55.00mg/kg. Conclusions: The monitor method was sensitive、accurate and precise for national standard foundation. [Keywords] Pesticide Residue, Organ-phosphorus Pesticide, Chinese Herb, gas chromatograph method 作者简介：邱绿琴，女，大学本科，主管中药师 ，长期从事中药调制和中药制剂方面研究工作。 随着中医药事业的发展，中医药在世界范围内的防病和治病作用受到越来越多的关注，而中药却不为国际承认，主要原因在于中国的中药及其制剂缺乏完备合理的质量控制标准，包括中药及其制剂有效成分（活性成分）质与量的控制以及中药及其制剂中有毒、有害成分（杂质）的种类和量值控制。所以制订中药及其制剂质量控制标准显得刻不容缓。 由于野生药材资源日渐枯竭，因此人