| Objective: To optimize the conventional processes in order to increse the effects of clarity and perfect its original quality standard, preliminary stability of the processes after amelioration was investigated on Xiaoer-Qingre-Lifei oral liquid.Methods: Using the retention rate of Chlorogenic Acid, Forsythin, Arctiin and Ephedrine Hydrochloride content as the index to track the metastasis rate of the active components and analysis of the specific reasons for differences in Xiaoer-Qingre-Lifei oral liquid key process. The chemical, instrumental and other technical integration analysis were using into the chemical composition of precipitations, study the effects of protein, tannin and pectin on clarity and stability of herb decoction. Turbidity was applied to measure the effects of clarity, and using the retention rate of active ingredient, tannin and solid content removal rate as the indicator to evaluate the use of chemical, membrane separation technology and high-speed centrifugal technology and other techniques to further improve product quality feasibility. Honeysuckle, Ephedra, Forsythia and Burdock on Xiaoer-Qingre-Lifei oral liquid were identified by TLC; The content of Chlorogenic Acid, Forsythin, Arctiin and Ephedrine Hydrochloride was determined by HPLC in the study of quality standard. Preliminary stability was investigated by long-term testing.ResuLts: The process of extraction, alcohol precipitation and concentration were the major reasons of active components loss, and reducing loss by process adjustment. The precipitations were divided into the black and the white. The black mainly composed of tannins, accounting for 80% of the total precipitations, the white was about 7%. The whiteprecipitation is a mixture with some hydrated calcium oxalate and hydrated calcium sulfate, and main phase is new hydrated compounds consist of a calcium carbonate as the main organic component and TCM complex. Oxidative polymerization of tannins is the main factor of clarity and stability of herb decoction. The formation of the white precipitation mainly result from saturation, pH and temperature of liquid. The black can be removed entiretily by regulate the process conditions, but the white in Xiaoer-qingre-lifei Oral liquid. Membrane technology in the best entry point was total mixed liquor contains syrup; ceramic membrane filtration was more efficient than vibration membrane, but the membrane separation technology makes ephedrine hydrochloride and chlorogenic acid content decreased. High-speed centrifugal technology loss of less active ingredient content, and like membrane technology can not completely remove the white. Through the chemical means to change the temperature, pH, and the supersaturation has a discovrery. When the temperature is 30℃±10℃, and the pH is neutral or lean to acidic, significantly reduced the amount of white precipitation and the stability phase markedly transformation as the supersaturation. The quality identification by TLC was specific,having a good separation and a clear spot in each thin layer plate. The method showed sample size showed a good linear relationship with in the range of 16.28μg~81.4μg of chlorogenic acid (r=0.9996, n=5). The average recovery was 100.31% with RSD=1.45%. Ephedrine Hydrochloride was linear with logarithm of the area in the range of 1.598~19.176μg of (r=0.9995, n=5). The average recovery was 99.91% with RSD = 1.17%. The calibration curve of forsythin was linear in the range of 0.13μg ~160.20μg (r=0.9998). The average recovery of forsythin was 99.43% with RSD=1.02% (n=6). The calibration curve of arctiin was linear in the range of 0.13μg~322.40μg (r=0.9997). The average recovery of arctiin was 99.66% with RSD=1.54% (n=6). Preliminary stability of the processes after amelioration were increased by long-term testing.ConcLusion: The technics amelioration of Xiaoer-Qingre-Lifei oral liquid was reasonable, practical. The evaluation methods are simple, specificity, reproducible and can be used in the quality control of compound huangqi changning granules. And the quality of the sample was steady as well. |
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