| Objective:To study the common condition of exogenous hazardous substances residual in Chinese herbal medicine(CHM). And establish a method to determine the exogenous hazardous substances residue in CHM which is in line with the international conventions and adapt to the domestic reality.Method:A method was found in the process of detecting the concentrations of pesticide and multi-residue in CHM, which is extracted by ethyl acetate/cyclohexane(V/V=1:1) then cleaned up by GPC and detected by GC-MS. The criterion curve the recovery and the precision are all quite well. At the scope of (92.5%～96.2%) when 0.375μg·ml-1 was added into the original medicine. high precision was showed In every repeated test, the recoveries'RSD0.85%～3.56% between every pesticide. This method was convenient, sensitive, accurate and suitable for detect the pesticide multi-residue in Chinese herbal medicine.To detect the quantity of the heavy metals in CHM,we established the method of Microwave Digestion with nitric acid and hydrogen peroxide,and determine by ICP-OES. The recovery and precision was nice (94.7%～97.2%) at the concentration of 0.4mg·kg-1 added to the sample.This method proved to have a good consistency, and is able to detect the CHM sample. StabilizlyIn Sulfur Dioxide test we had referred the method of sulphur dioxide in food detection, Distillation and colorimetry was checked for determine Sulfur Dioxide. In our test the recovery of distillation and colorimetry was 93.5% and 95.4%, the consentrition of 100μg·ml-1 of the standard was added equal to original medicine.The colorimetry recoveries' RSD% was 0.9979. the result showed that the above-mentioned method is able to detect the sulfur dioxide in CHM.Results:In the pesticide residue detecting, only4 samples checked out in 94 samples,among them two Ligusticum chuanxiong exceed commen standards. It can be seen that pesticide residue condition is not seriouse in the CHM. In the heavy metals detecting, 40.4% are above the standards. the proportion of the disqualified was unexpectedly reached to 61.9% in Ligusticum chuanxiong samples in Cd test. In all of the items which exceeds allowed figure, almost is Cd,there are only 4 Hg items in Coptis chinensis samples. the reason of this phenomenon is waiting for further studies. The sample sulfur dioxide discovering 23.4% in detecting goes beyond normal standard, the sample that checked out except were having going beyond standard other outside Ligusticum chuanxiong, that more Ophiopogon japonicus and Rheum officinale's sulfur dioxide was going beyond standard, deduction to going beyond standard is aroused by using sulphur suffocating in the treating process.After inquired planting base in Chongqing Shizhu and Sichuan Pengzhou., we kown the fundamental condition that our country CHM produces the GAP base the CHM. As a result of GAP implementation and government and local lead enterprise's cooperation development. The CHM planter processing gradually is moving towards the modernization though exist such problems, has built the good foundation for produce the qualified CHM.Conclusions:This experimentation establishes the method of Pesticide detect Residue and heavy metals and Sulfur Dioxide in CHM, which should be suitable for the CHM Exogenous Hazardous Substances examination. |
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