Application Of Chromatography-mass Spectrometry In Drug Quality Control

The quality of drugs, being directly related to people's physical and mental health, affecting the sustainable development of the economy and the society, has already caused the great attention of the country and the extensive concern of the whole society at present. As China joined the WTO, foreign countries raised the drug inspection standards higher towards our country in the trade, especially for the traditional Chinese medicine. As we known, most contaminants in drugs have the potential biological activity, and some of them affected mutually with the drugs. They can affect the medicine security and the efficiency, even produce the toxic effect. Therefore, the quality control of drug, especially the analysis and evaluation of impurities, degradation products, prohibitive additives and pesticide residues, etc. in drugs, is being paid more and more attention.Analytical method standard is the key factor of affecting the examination result, which is also the basis and criterion of the drug quality control. The international society attaches much importance to the technological research of drug quality inspection, and then establishes the advanced and scientific analytical method standard on its base. The chromatography-mass spectrometry, associated with the high separating power of the chromatography, the high sensitivity, the great structure analyzing ability, the high specificity and the versatility, and the high analyzing speed of MS, has become the effective tool in this domain. Besides improving the inspection methods and controlling the contaminant level, the more important thing of guaranteeing the drug quality is taking appropriate measures to reduce the contaminant content. Consequently, the combination of the inspection and control can finally enhance the quality of drugs.A high performance liquid chromatography-diode array detection-electrospray ionization tandem mass spectrometry method was developed for analysis and identification of impurities in lovastatin. Lovastatin and impurities were separated using acetonitrile-water (containing 0.1% acetic acid) (65:35, v/v) as mobile phase. The elutes were detected with diode array detector and ion trap mass spectrometer in positive mode. The UV, MS and MS~2 spectra of each chromatographic peak wereobtained. Then the [M+H]+ ions and their MS2 spectra were used for determining the molecule mass and side-chain. According to analyses of the UV, MS and MS2 as well as the comparison with the published literature, the structures of ten impurities were identified. At last, three impurities were separated by column chromatography and preparative thin layer chromatography, and confirmed by NMR technique. The results indicated that the HPLC-DAD-MS method could be effectively applied to perform identification of impurities in lovastatin.The characteristic and effect factors of the degradation of organochlorines, organophosphorus and pyrethroid and alkaloids in Radix Sophorae Flavescentis by hydrogen peroxide (H2O2) were investigated. The results showed that H2O2 had highly activity in degrading organophosphorus and pyrethroid, but had less activity to organochlorines. The degradation processes of organophosphorus and pyrethroid followed first-order kinetics equations, influenced by the pH value, the concentration of H2O2 and reaction time. Also, the contents of alkaloids in Radix Sophorae Flavescentis were changed, but the changes were not obvious after treatment less than 6 hours with 3mL/L H2O2 under neutral condition.