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Basic Study On Quality Control Of Microcos Paniculatae

Posted on:2013-06-15Degree:MasterType:Thesis
Country:ChinaCandidate:P LuFull Text:PDF
GTID:2234330371998270Subject:Drug analysis
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Microcos Paniculatae L.one of the genuses of Tiliaceae Microcos. Microcos Paniculatae L. mainly distributed in our country Guangdong Hainan Guangxi Yunnan etc. Especially in Guangdong Province-wide distribution production resource-rich. The Yangjiang and Ganjiang are the leading producer of Guangdong Province. Microcos Paniculatae L., level in nature and acid in taste, non-toxic. It has the abilities of activating, digestion, and stimulating the appetite. It attend consumptive cold, sore throat, abdominal distension and jaundice. Microcos Paniculatae L. is a famous Chinese medicine and widely distributed in south China for summerish tea.This topic as the research object of Microcos Paniculatae L. Using the modern analysis method. According to quality control of Microcos Paniculatae L. and researches on safety. Set up quality control standards, pesticide residue content and heavy metal content of Microcos Paniculatae L’detection methods. The research content and the results are as follows:1、On the basis of the existing literature optimize the TLC of Microcos Paniculatae L. Thereas four spots from the Paniculatae L. were narcision. vitexin. Invitexin and kaempferol by the TLC in365nm with (Ac)EtOH:butanone:formic acid:water(5:3:1:1) as developing solvent and with5%AlCl3solution as chromogenic reagent.2、Chromatographic fingerprint analysis is a rational approach for quality assessment of traditional Chinese herbal medicine. In this topic, Try to set up the chromatographic fingerprint of by high performance liquid chromatography. The chromatographic condition was described as follow:Separation was performed on a Kromasil Ci8(5um,4.6mm×200mm) column. Mobile phase A was methanol, while mobile phase B was water. Linear gradient elution was performed with in a100min running time and its sequence was as follow:The beginning with17%of mobile phase A and83%of mobile phase B, then the mobile phase A to B ratio was gradually change to42%~58%at40min, which was maintained for10min.The flow rate was set to1.0ml/min and the UV detector was set to278nm. The column temperature was set to30℃. Fourth common peaks on the HPLC fingerpints.3、A HPLC assay was developed for determination of vitexin and narcision in the herba of Microcos Paniculatae L. The chromatographic condition was described as follow: Separation of tow compounds were achieved on a Kromasil Ci8(5um,4.6mm×200mm) column with mobile phase consisting of methanol and water. The column temperature was at30℃. Gradient elution with the flow rate of1.0ml/min. The fluorescence detecting wavelength was set at339nm. After the method validation, there were two good linearity over the range of0.1~4μg with a correlation coefficient greater than0.999, respectively. Good precision and stability were obtained in this method with RSD little than2.0%. While the recovery ranged from95%to100%. This method was successfully applied for determination of Microcos Paniculatae L.4、Using the thechnology of infrared spectroscopy, By means of get the fingerprint of infrared and second-order derivative to analyze Microcos Paniculatae L.The results show that the infrared spectroscopy can identify Chinese thraditional Drogs directly and fast.5、To assay the contents of5heavy metal of Cu, As, Cd, Hg, Pb in Microcos Paniculatae L. by microwave digestion with inductively coupled plasma mass spectrometry(ICP-MS). With germanium Ge, In, and Bi as the internal standard substance. The contents of the5heavy metals of Cu, Pb, Hg, As, and Cd were detected with ICP-MS. Simultaneously after the samples of Microcos Paniculatae L. was trected by microwave digestion. The nation standard substance of orange leaves(GBW10020) was used to estimate the accuracy of method. For all of the analyzed heavy metals. The correlation coefficient of the calibration curves was over0.9990, RSD were in the rage of1.1%~11.6%and the recovery rates of the procedure were97.9%~108.9%.6、Gas chromatography was established for9organochlorine pesticide residue in Microcos Paniculata L. The sample was infilated with water and extracted ultrasorcically with hexane. The extract solvent was purified by concentrated sulphuric acid DB-1701capillary column was used to separate the sample. GC-ECD was applied to determine the residues of oraganochlorine pesticide. Results:The perecentage recoveries were ranged from78.1%to97.8%and RSD were from2.4%to8.8%.
Keywords/Search Tags:Microcos Paniculata L., quality standard, TLC, content determination, fingerprint, infrared spectroscopy, contents of heavy metal, organochlorine pesticideresidue
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