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ObjectiveTo evaluate the metabolic stability of lucidin by incubating liver microsomes and liver S9 from 4 species， and to compare the species differences in metabolism of lucidin in vitro. MethodA qualitative and quantitative method of lucidin based on ultra-high performance liquid chromatography-high resolution mass spectrometry （UHPLC-HRMS） was established and verified. Lucidin was incubated with rat， mouse， beagle dog， human liver microsomes and liver S9 to investigate the metabolic stability parameters， metabolites， metabolic pathways. ResultHepatic clearance （CLh） of lucidin was in order of mouse>rat>beagle dog>human in both phase Ⅰ and phase Ⅱ incubation system. Its metabolic stability was good in rat， beagle dog and human， while it showed metabolic instability and moderate metabolic stability in mouse microsomes and liver S9， respectively. A total of 5 metabolites were rapidly identified， including 3 oxidation metabolites of phase Ⅰ and 2 sulfation metabolites of phase Ⅱ. The production rate of metabolites was consistent with the results of metabolic stability. ConclusionThe established UHPLC-HRMS is simple and specific， which can be used for the study on the metabolic stability and metabolites of lucidin. Its metabolic stability and metabolite production rate in vitro are significantly different among species， the metabolic characteristics of rat and beagle dog are similar to human， which provides an important reference for subsequent research in vivo， safety evaluation and animal model selection of lucidin.
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OBJECT IVE To provide reference for the improvement of the quality standard for Niushanggui capsules. METHODS Based on the previous quality standard ，thin-layer chromatography （TLC）identification methods were established for Angelicae dahurica and Anemarrhenae asphodeloides . High performance liquid chromatography （HPLC）method was established to determine the contents of 5 components simultaneously ，such as mangiferin ，prim-O-glucosylcimifugin，naringin，neohesperidin and 5-O-methylvisammioside. The limits were confirmed. RESULTS TLC chromatogram of Niushanggui capsules showed the same color spots in the same position as the corresponding （mixed）substance control or reference medicinal material of A. dahuricae and A. asphodeloides ，while the negative samples had no interference. The linear range of mangiferin ，prim-O-glucosylcimifugin， naringin，neohesperidin and 5-O-methylvisammioside were 7.98-127.63，6.74-107.84，53.06-848.96，39.31-628.90，13.54-216.62 μg/mL，respectively（all r＝0.999 9）. RSDs of precision ，stability（24 h）and repeatability tests were all no more than 1.20％（n＝ 6）. The average recoveries were 95.00％，105.16％，97.16％，101.00％ and 104.97％（RSD≤1.50％，n＝6）. In 4 batches of samples，the average contents of the above 5 components were 0.842，0.696，6.951，5.755 and 1.106 mg/g respectively ；the limits of A. asphodeloides ，Saposhnikovia divaricata and Citrus aurantium were based on the contents of mangiferin ，the total content of prim-O-glucosylcimmifugin and 5-O-methylvisammioside，naringin and neohesperidin ，which would not be less than 0.42，0.90 and 6.36 mg/grain，respectively. CONCLUSIONS TLC identification methods of A. dahurica and A. asphodeloides and the content determination methods of 5 components as mangiferin in Niushanggui capsules are established in this study ，and the limits of A. asphodeloides ，S. divaricata and C. aurantium are confirmed.
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Objective To establish the analytical method for fingerprint of Aristolochia manshuriensis by HPLC-DAD-ESI/MS,which can be used as the basis for quality control of the drug and for the further studies on kidney toxicity metabolite.Methods Samples A.manshuriensis from different habitats were extracted by 75% methanol and analyzed by HPLC-DAD-ESI/MS,whose chromatographic fingerprints were established.Two ways to calculate the similarity were selected to compare the results by determining the common peaks.Results There were 30 main characteristic components in A.manshuriensis.The HPLC-DAD-ESI/MS fingerprint of the 30 common peaks was established preliminarily.The samples of A.manshuriensis from different habitats was found having a good similarity,and the range of similarities for 24 balches of A.manshuriensis were 0.871—0.998.Conclusion The method is reliable,accurate,and of good stability,and can be used for the quality control and variety identification of A.manshuriensis.
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Objective To establish a method for determining cinnamaldehyde in Zegui Longshuang Capsules. Methods A C18 column was used with Acetonitrile-Water (30∶70) as the mobile phase,and the detection wavelength was at 290 nm. Results The calibration curve of cinnamaldehyde was linear from 0.010 ?g to 0.507 ?g,and r=0.999 9. The average recovery was 98.55 %with RSD being 2.06 %. Conclusion This method is proved to be accurate and reliable,and can be used to control the quality of Zegui Longshuang Capsules.
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AIM:To study the ingredients of sediments from Xiexin Decoction(XXD)(Radix et Rhizoma Rhei; Radix scutellariae and Rhizoma coptidis) with the method of LC/MS2. METHODS:A C 18 column was used,with acetonitrile-acetate buffer as mobile phase,and the online detection wavelength was 270 nm. RESULTS:The ingredients of sediments from XXD were nearly the same as its supernatant fluid,There were the similarities between the solubilities of sediments from XXD in artificial gastric juice and in artificial intestinal fluid. CONCLUSION:In clinical trials we should pay much attention to this fact that sediments from XXD and its supernatant fluid have similarly importance.