| Chinese materia medica preparation, which can be called the national treasureand quintessence of China, is one of the pharmaceutical preparations based onChinese herbal medicines (CHMs). Recently, Chinese materia medica preparation hasbeen widely used in clinical departments because of their natural ingredients,mildness, effectiveness and slight side effects. On the other side, the safety andquality of this kind of medicine has caused wide public concern.The growing demand of Chinese materia medica preparation results in theartificial cultivation of CHMs, and the cultivation relying on various kinds ofpesticide to prevent, repel or mitigate the effects of pest. However, the CHMs have ahigh risk of pesticide contamination during their cultivation, storage andmanufacturing processes. The pesticide residues in CHMs may further to contaminateChinese materia medica preparation and seriously harm for the human health. Thus,developing rapid, simple, effective and sensitive method for the simultaneousdetermination of pesticide residues from different forms of Chinese materia medicapreparation has an important realistic significance.In this work, using GC and GC-MS/MS technique, new analytical methods onthe determination of pesticide residues in various forms of Chinese materia medicapreparation were developed. These methods have been applied to the analysis of realsamples and have already obtained good results. The main achievements of our studyare as follows:1. A new method for the simultaneous determination of14organophosphoruspesticides (OPPs) in Shiduqing pills was established. Samples were extracted by ethylacetate. Cleanup of extracts was performed with graphitized carbon black. Thedetermination of pesticides in the final extracts was determined by GC-FPD. Underoptimized conditions, except for dimethoate, the recoveries of13organophosphoruspesticides were from80.4%to114.5%, at spiked levels0.1mg/kg and0.5mg/kg, andRSDs range from0.6%to12.4%. The limits of detection (LODs) oforganophosphorus pesticides were0.03~0.05mg/L. The method could meet therequirements of pesticide residue analysis and could be effectively used to analyse the 14organophosphorus residues in Shiduqing pills saled.2. A new multi-residue method for the simultaneous determination of11OPPs inShuanghuanglian oral liquid and Antivirus oral liquid was proposed. The oral liquidsamples were extracted by mixture of acetone and n-hexane through a one-stepextraction procedure, without further clean-up step, the extract was directly identifiedand quantified by GC-MS/MS after dryed and diluted in a constant volume. Underoptimized conditions, excellent linearities (0.01~0.2mg/L, with the correlationcoefficient>0.9997), low LODs in Shuanghuanglian oral liquid (0.04~1.22μg/L)were achieved with acceptable recoveries (70~120%) and RSDs (less than13.3%) formost pesticides at three spiked levels (10,20,50μg/L). The presented method couldmeet the requirements of pesticide residue analysis and could be useful for the routineanalysis of11OPPs in Shuanghuanglian oral liquid and Antivirus oral liquid.3. A new method was developed for the the simultaneous determination oforganochlorine and pyrethriod pesticide residues in Six ingredient rehmannia pillsand Xiaoyao pills. Samples were extracted by ethyl acetate. Cleanup of extracts wasperformed with graphitized carbon black. The determination of pesticides in the finalextracts was determined by GC-MS/MS. Under optimized conditions, except forhexachlorobenzene, the recoveries of17pesticides were from75.5%to114.6%, atlow, medium and high spiked levels, and RSDs were less than10.0%. The LODs of18pesticides in Six ingredient rehmannia pill ranged from0.02to8.82μg/kg. Themethod could meet the requirements of pesticide residue analysis and could beeffectively used for routine analysis of the organochlorine and pyrethriod pesticideresidues in Six ingredient rehmannia pills and Xiaoyao pills saled. |
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