| Objective:1 To provide the basis for the improvement of quality standards and quality control of raw herbs through the development of its quality control system with multiple indexes.2 To provide the basis for the priority of raw materials on Mugua dispensing granules through quality analysis of the decoction pieces.3 To optimize the extraction process of Mugua dispensing granules by the comparative study on two kinds of extraction process.4 To make a draft about quality standard for Mugua dispensing granules and to control its quality effectively.5 To study the quality correlation of raw herbs- decoction pieces-extract- dispensing granules of Chaenomelis Fructus, and to provide a scientific and effective basis for its quality control in whole process of production.Methods:1 TLC experiments were performed to identify 10 batches of raw herbs,and HPLC was applied in determinating the triterpenoid acids and water-soluble organic acids.Some tests(H2O,total ash, p H and Et OH extract) were done.Extract the samples with dilute alkali and ultrasonic extraction after immersion, detecting the content by using the technology of potential residual titration,and malic acid(C4H6O5) as control article.Titration test of substance(malic acid, citric acid, benzoic acid and phenol) were used for the investigation of potential direct titration and residual titration. The correlation of total organic acids, its monomer and p H value were analyzed by using the scatter plots and Pearson correlation coefficient.2 TLC was used to identify decoction pieces were analyzed for decoction pieces, and HPLC was applied in its determination of water-soluble organic acids and triterpenoid acids.Some tests(H2O,total ash, p H and Et OH extract) were done.3 Optimum extracting process was conducted by the compaison on the content of organic acids in water decoction and extract.4 TLC was used to identify Mugua dispensing granules,the technology of potential residual titration was applied to detecte the content of total organic acids, HPLC was conducted to determinine the content of water-soluble organic acids and triterpenoid acids. The specific chromatograms were established by HPLC.5 The quality correlation of raw herbs- decoction pieces-extract- dispensing granules was studied by HPLC specific chromatograms.Results:1 10 batches of raw herbs showed the same color spots and fluorescent spots with control medicine and oleanolic acid on the corresponding position. The content of water,total ash, Et OH extract met the pharmacopoeia. PH value of 4 batches of them,oleanolic acid and ursolic acid in total 5 batches of them were less than the specified value. The content of water-soluble organic acids and total organic acid were in the ranged of 1.110%~2.233% and 18.50%~32.03%,respectively. Potential direct titration method can not accurately determine the content of benzoic acid, and potential residual titration method can accurate determine the content of benzoic acid, malic acid and citric acid. This method can eliminate the interference of deep color on extraction, the titration curve has obvious jump, and the total content of organic acid in the sample was higher than that of distilled water and 75% ethanol. This method has the advantages of simple operation, stable and reliable.There is a significant correlation between the content of total organic acids and p H value, water-soluble organic acid, but the correlation was not obvious with triterpenoid acids.2 Decoction pieces, control medicines and ursolic acid had the same color on the spots and fluorescent spots in TLC experiment.The content of total ash met the requirements of Pharmacopoeia, the content of water in 1 batches was higher than the specified value,p H value of 5 batches were lower than the specified value. The content of extract and water-soluble organic acids were in the range of 25.11%~39.77%,and 1.813%~2.697%,respectively.The total content of oleanolic acid and ursolic acid was in the range of0.344%~0.518%.3 The content of total organic acids and the total content of oleanolic acid and ursolic acid in three batches of extract were 15.81% and 0.513%, which were greater than that of water decoction. The content of water-soluble organic acids in extract was 0.528%,which was less than that of water decoction(1.386%).4 The quality standard draft of Mugua dispensing granules was developed: oleanolic acid and ursolic acid were identified in dispensing granules, the water content shoud not be more than 6.0%. the content of total organic acids, water-soluble organic acids,oleanolic acid and ursolic acid in 1g dispensing granules shoud not be less than 192.0mg,35.22 mg and 5.0mg, respectively. The HPLC specific chromatograms of Mugua dispensing granules was established,5 characteristic peaks were indicated,it require that the relative retention time of the characteristic peaks should be in the range of ±5% of specified value.Specified value: 0.23(peak 1),0.25(peak 2),0.85(peak 3),1.00(peak S),1.63(peak 4)。5 The peak shape and peak number of raw herbs are basically consistent with decoction pieces,extract and dispensing granules. And the similarity between their standard specific chromatograms were both greater than0.90.Conclusion:This paper set up a quality control system with multiple index of raw herbs and decoction pieces,which can provide a basis for the improvement of quality standards and optimization of Mugua dispensing granules.The extraction process of ethanol and water compared with the traditional water extraction process effectively improves the extraction rate of fat-soluble components,such as oleanolic acid and ursolic acid.This process can also extract water-soluble ingredients, and keep the pharmacodynamic material basis consistent with decoction pieces.The established qualitative and quantitative method has the advantages of convenient operation, accurate and reproducible and can control the quality of Mugua dispensing granules.The newly developed specific chromatograms of Mugua dispensing granules was traceable to its raw herbs,decoction pieces and extract.This method could be used for the quality control of Mugua dispensing granules in whole process of production. |
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