【作者】 廖华军；

【导师】 郭素华；

【作者基本信息】 福建中医学院 ， 中药学， 2005， 硕士

【摘要】 目的:通过对我省主要中成药中农药残留和重金属含量的测定,了解我省中药中农药残留及重金属含量情况,为中药生产中的质量控制和临床中的安全用药提供科学依据,为我省中药出口和中药现代化发展提供参考依据。 方法与结果: 第一部分:闽产主要中成药中有机氯农药残留含量的测定。选择福州、厦门、漳州、建阳等地区部分主要中成药,对其有机氯农药残留含量的测定,样品通过丙酮+水超声提取,二氯甲烷萃取,加入氯化钠使有机相与水相分层,浓硫酸净化,离心,取上清液浓缩、定容。采用交联OV-1701石英毛细管色谱柱分离样品,ECD检测农药六六六、滴滴涕、五氯硝基苯的含量。实验加样平均回收率:83.01%～97.72%,RSD:2.94%～6.17%。各被测样品中有机氯农药残留含量较低,符合国家标准。 第二部分:闽产主要中成药中有机磷农药残留含量测定。样品用丙酮+水恒温振荡提取30min,用正已烷+丙酮,乙酸乙酯;丙酮+乙酸乙酯:丙酮+甲醇梯度洗脱硅胶小柱净化样品,汇集全部滤液经旋转蒸发仪45℃水浴浓缩近干,定容至1ml。用HP-1701石英毛细管柱,程序升温法分离样品,NPD检测器检测敌敌畏、甲胺磷、乙酰甲胺磷等有机磷农药含量:实验加样平均回收率:80.1%～95.3%,RSD:2.5%～6.6%:所测样品都不含有有机磷农药残留。 第三部分:闽产主要中成药中重金属的含量测定。①铅和镉,精密称取样品于瓷坩埚中,电热板上炭化,移入马弗炉灰化:用硝酸(0.5ml/L)将灰分溶解,用滴管将样品消化液洗入容量瓶中,少量多次洗涤坩埚,洗液合并于容量瓶中并定容至刻度,混匀备用;②汞,精密称取样品,置于消化装置锥形瓶中,加入硝酸,硫酸:小火加热回流,冷却,将消化液过滤,用少量水洗锥形瓶、滤器,洗液并入容量瓶内,加水至刻更多还原

【Abstract】 Objective :Through determinatin of pesticides residues and heavy metal in the famous Chinese Traditional Patent medicine of our province, situations of the pesticides residues and content of heavy metal in the Chinese Traditional Patent medicine of our province are understood,which may offer scientific basis for the fact that quality control in production and security of use medicine in clinical and offer scientific reference basis to export Chinese Traditional medicine and achieve Chinese Traditional medicine modernization for our province.Method and result: First part,Determinatin of pesticides residues of organic chlorine in the traditional Chinese Patent medicine in Fujian.,Chinese Traditional Patent medicine were selected from Fuzhou , Xiamen , ZhangZhou , Jianyang ,etc. the sample is drawn through the the mixed solvents of acetone and distilled water by supersound, extract with Methylenechloride, add sodium chloride makes organic and water divide layer, purified by concentrated sulfuric acid, centrifugated, take upper clear liquid concentrated , fixed volume. separated by unite ov-1701 quartz capillary chromatogram The average recovery rate 83. 01%-97. 72%,RSD: 2. 94%- 6. 17%. The content of organic chlorine pesticide is lower accord with the national standards.Second part: determination of Organophorous pesticide residue in Chinese Traditional Patent medicine in Fujian.the sample are draweded through the mixed solvents of acetone and distilled water in the condition of constant temperature by vibrator, purge sample with silica gel columella by gradient elution adsorbent system of normal hexane and acetone, acetic ester, the mixed solvent of acetic ester and acetone, the mixed solvent of acetone and methanol,converged eluting liquid , concentrated in water bath close to dry by rotary evaporimeter, hold it to 1ml definitely. separated by HP-1701 quartz capillary column, detected by NPD . The recoveries were 80.1%~95.3% with RSD 2.5%~6.6%, The range of detectable limits were 5.21×10~-3~3.26×10~-2 ng .dichlovos, Methamidophos, Acephate and theother eight kinds of pesticides aren’t found in the sample examined.Third part:, Determination of Heavy Metal in Chinese Traditional Patent medicine in Fujian, the sample accurately weighed was placed in crucible, carbonizing on zoom type electric hot plate with little current to no smoking, then migrate to massmann furnace ashing; the ash was dissolved in 0.5 nitric acid, solution was migrated to 10-25ml measuring flask, Washing crucible repeatedly, amalgamating washing liquor to measuring flask and fixed capacity to scale, mixing evenly ,the lead and cadmium are detected by atomic absorption spectrometers. 1.00-5.00g sample weighed was placed to conical flask, added 45ml nitric acid and 10ml sulphuric acid, heated refluxing 2hour, colded. the solution is filted to measuring flask, washing conical flask, filter, washing liquor was converged to measuring flask, adding the water to scale, mixing evenly, mercury is detected by Cold atomic fluorescence spectrophotometer parameter; the 1.00-5.00g sample was placed into beaker, adding 10ml nitric acid, mixed thoroughly ,added 5ml sulphuric acid, left to stand for 24h; the next day ,added 2.5ml perchloric acid, heated at low temperature, add 10ml mixing solution of 5% ascorbic acid and 5% thiocarbamide, translated to measuring flask. Arsenium is detected by atomic fluorescence spectrophotometer parameter, the percentage of theHeavy Metal in the sample detected in this experiment: the lead is 0, cadmium is 0 ,mercury is 53.19% and Arsenium is 2.13%.Conclusion Organochlorine pesticides is low in the sample examined, indicating Chinese Traditional Patent medicine in our province organic chlorine polluted lightly by organochlorine pesticides, no Organophorous pesticide are found the sample,Organic chlorine , organic phosphorus agriculture chemical have a little effect on health in some Chinese Traditional Patent medicine of our province, mercury and arsenic content exceed standard in some Chinese Traditional Patent medicine, it must take measures further to reduce content. Guarantee that it is healthy to use medicine.更多还原