Taking Pudilan Xiaoyan Oral Liquid as a demonstration, the effective delivery of quality markers in alcohol precipitation of Chinese medicine oral liquid preparations was studied. With the transfer rates of adenosine, corynoline, cichoric acid, baicalin, and wogonin as evaluation indexes, the effect of the density of concentrate before alcoholic precipitation, volume fraction of ethanol, stirring speed, temperature of concentrated solution, stirring time, alcohol concentration, alcohol precipitation time, alcoholic precipitation temperature, alcohol addition rate, and the pH of concentrate on the alcohol precipitation process was investigated by Plackett-Burman trial design, thus obtaining the key factors that influenced the alcohol precipitation process. The key factors were further optimized by Box-Behnken design to determine the optimal alcohol precipitation conditions. When the density of concentrate before alcoholic precipitation was 1.12 g·mL~(-1), the pH of concentrate was 6.86, and the alcohol concentration was 50.00%, the transfer rates of baicalin and wogonin were 91.86% and 87.78%, respectively. When the density of concentrate before alcoholic precipitation was 1.13 g·mL~(-1), the concentration of alcohol was 74.50%, and the alcoholic precipitation temperature was 17.0 ℃, the transfer rates of adenosine, corynoline, and cichoric acid were 85.95%, 71.62% and 83.19%, respectively. The method of optimizing alcohol precipitation techniques and determining the parameters of Pudilan Xiaoyan Oral Liquid by response surface methodology is reasonable and feasible, which provides guidance and experience for the effective delivery of quality markers in Chinese medicine oral liquid preparations.
Drugs, Chinese Herbal ; Ethanol ; Adenosine ; Chemical Precipitation

OBJECTIVEWater content in concentrated extract (WCCE), the concentration of ethanol used in precipitation (CEA) and the quantity of ethanol added( QEA) are three important variables in the first ethanol precipitation of Danshen injection. In this work, the relationships between the three variables and total solid removal, Danshensu (DSS)retention and DSS purity were investigated.

METHODExperiments according to central composite design were carried out and mathematical models were developed.

RESULTThe models were accurate and predictive. The relative deviations between prediction results and experimental results were less than 3%. The influences of the three variables were discussed with a response surface method. The decrease of WCCE and the increase of CEA both caused more precipitation and increase the purity of DSS. However, more loss of DSS was observed. The increase of QEA increased total solid removal. DSS retention and DSS purity increased first and then decreased when QEA increased.

CONCLUSIONThis result suggests the addition of ethanol should be optimized according to WCCE and CEA to obtain better supernatant

Chemical Precipitation ; Ethanol ; chemistry ; Models, Statistical ; Reproducibility of Results ; Salvia miltiorrhiza ; chemistry ; Water ; chemistry

The theoretical basis of the alcohol precipitation process control was provided, the alcohol precipitation was optimized and the relationship equation was got. The monod glycoside, loganin and paeoniflorin were used as the evaluation indexes to determine the impact factors of alcohol precipitation techniques of Liuwei Dihuang decoction by the Plackett-Burman experimental design and the levels of non-significant factors were identified. Then, Box-Behnken response surface methodology was used to research and discuss the critical process parameters influence the effect of alcohol precipitation and draw interaction between key process parameters and the correlation equation with index components. Through the establishment and solving the quadratic regression model of composite score, the optimum preparation conditions of alcohol precipitation techniques of liuwei were as follows: stirring speed was 580 r x min(-1), standing time was 17 hours, alcohol concentration was 34%, the density of Liuwei Dihuang decoction was 1.13. The response surface methodology for optimized alcohol precipitation techniques of Liuwei Dihuang decoction is. reasonable and feasible.
Chemical Precipitation ; Chemistry, Pharmaceutical ; methods ; Drugs, Chinese Herbal ; chemistry ; Ethanol ; chemistry

Introduction: The need for gama \u2013 globulin, especially gama - globulin - anti \u2013 HBs, is huge in Vietnam. A number of patients cannot to afford use them due to the high price as they are imported. Meanwhile, Vietnam has high quality input sources for producing gama \u2013 globulin. \r\n', u'Objectives: To study the production process of gama - Globulin from Human Plasma and Standard gama - Globulin with Rich of Anti \u2013 HBs. \r\n', u'Subjects and method: 168 samples of human plasma from voluntary blood donors, which had been screened with for transfusion transmittable infections (TTLs), were chosen as plasma with rich of anti - HBs. The plasma with anti - HBsAg was precipitated with ethanol 25%, pH 6,9 to gain gama - globulin with rich anti - HBs, which was dried by Dutch Ly - 3 - TTE machine. Activation of anti - HBs gama - globulin was identified by a standard method of the degree of antibody specific for anti - HBsAg kit of BIORAD, \r\n', u'Results: The purity of the gama - globulin achieved was 93%, which was almost equal with the results of some foreign researchers (7.8), the activation of anti - HBs was 1:128 dilution degree. The productivity of gama - globulin gaining from 1 litter plasma was 6.0 gram. This new issue was first demonstrated in Vietnam. \r\n', u'Conclusion: We can domestically produce anti-Bs gama - globulin with high degree of activeness (1:128) from human plasma by the precipitating method with ethanol, pH and low temperature. \r\n', u'
Human plasma ; gama - globulin - anti - HBs ; Precipitation of ethanol ; pH and low temperature

OBJECTIVETo study effect of alcohol concentration in water extraction and alcohol precipitation on the preparation of effervescent tablets of Banlangen.

METHODEffects of different concentrations of alcohol precipitation on the Banlangen extract rate, metastasis rate of index components, extract properties of powder, preparation process were investigated, respectively.

RESULTAlcohol concentration on the Banlangen extract rate, metastasis rate of adenosine, extract the amount of saturated moisture, effervescent disintegration time of no significant impact, but spray drying process, dry granulation process.

CONCLUSIONAlcohol concentration has a significant effect on the preparation of effervescent tablets of Banlangen in the process of water extraction and alcohol precipitation, It suggest that the choice of concentration of alcohol precipitation should be based on experimental purposes, the entire preparation process of the system test results.

Chemical Precipitation ; Drugs, Chinese Herbal ; chemistry ; Ethanol ; chemistry ; Tablets ; chemistry ; Technology, Pharmaceutical ; methods ; Water ; chemistry

OBJECTIVETo suggest a method for discriminating quality control indicators of concentrated solution before traditional Chinese medicine ethanol precipitation.

METHODThe second ethanol precipitation (SEP) of Guanxinning was taken as an example, with the concentrated supernatant of first ethanol precipitation (CSFEP) prepared with same dry matter content and the same amount of ethanol as raw materials, to conduct the ethanol precipitation test under the same conditions. The experimental data was analyzed by stepwise regression and partial least squares regression. Both of them selected the parameters which affect phenolic compounds retention ratios in SEP supernatant as the key indicators.

RESULTPhenolic compounds contents in SEP supernatant were mainly affected by the contents of danshensu, caffeic acid and salvianolic acid B in CSFEP.

CONCLUSIONThe discrimination method can be used to discover key quality control indicators of concentrated solution before ethanol precipitation.

Chemical Precipitation ; Ethanol ; chemistry ; Medicine, Chinese Traditional ; standards ; Quality Control ; Solutions

Astragalus polysaccharide has been widely used in food and medicinal industry owing to its health-promoting properties. In order to characterize better the relationship among molecular weight, structure-activity and activities, a simple method was used different concentration of ethanol including 30% (PW30), 50% (PW50), 70% (PW70), 75% (PW75), 80% (PW80) and 90% (PW90) to precipitate Astragalus polysaccharides into different molecular weight. As a result, PW90 showed smooth surface and the strongest antioxidant activity among these six fractions (P < 0.05). In conclusion, graded ethanol precipitation was a simple method to separate Astragalus polysaccharides into different molecular weight with different antioxidant activity fractions.
Antioxidants ; pharmacology ; Astragalus Plant ; chemistry ; Chemical Precipitation ; Ethanol ; chemistry ; Polysaccharides ; chemistry ; pharmacology

OBJECTIVETo investigate the optimal alcohol precipitation parameters for extract of Carthamus tinctorius.

METHODSThe effects of different factors on the transfer rate of hydroxy safflower yellow A (HSYA) was studied via single factor experiments, including the final alcohol concentration of the liquor, the speed of stirring, the initial density of the extract, the temperature and the pH of the liquor. Based on the results of single factor experiments, the final alcohol concentration of the liquor, the speed of stirring, the initial density of the extract and the pH of the liquor were studied by an orthogonal test and a multiple guidelines grading method, and the transfer rate of HSYA, the yield and the purity of extract in the supernatant were used as comprehensive evaluation index.

RESULTThe optimal alcohol precipitation process of Carthamus tinctorius extract was as follows: the final alcohol concentration of the liquor 50%, the speed of stirring 500 r/min, the initial density of the extract 1.15 g/ml and the pH of the liquor 5.0.

CONCLUSIONThe proposed alcohol precipitation process is convenient and steady with high transfer rate of HSYA, high yield and purity of extract in the supernatant.

Carthamus tinctorius ; chemistry ; Chemical Precipitation ; Ethanol ; chemistry ; Plant Extracts ; isolation & purification

Near infrared (NIR) spectroscopy as a kind of rapid process analysis technology has been successfully applied in Chinese medicine pharmaceutical process. In this research, the technology was adopted to establish the rapid quantitative analysis models of main indicators from the Lonicera japonica and Artemisia annua alcohol precipitation process of Reduning injection. On-line NIR spectra of 142 samples from alcohol precipitation process were collected and the content of main indicators for each sample were detected through off-line HPLC. With eliminating outliers, determination of spectra pretreatment method and selecting optimal band, the NIR quantitative calibration model for each indicator was established using partial least squares (PLS). These models were used to predict the unknown samples from precipitation process of Reduning injection to achieve the goal of rapid detection. The results showed that the models were ideal. The correlation coefficients of models for neochlorogenic acid, chlorogenic acid, 4-O-caffeoylquinic acid and secoxyloganin were 0.973 872, 0.985 449, 0.975 509 and 0.979 790, respectively and their relative standard errors of prediction (RSEP) were 2.922 49%, 2.341 37%, 2.930 40% and 2.184 60%, respectively. This study indicated that the NIR quantitative calibration model showed good stability and precision, and it can be used in rapid quantitative detection of main indicators of efficacy in order to on-line monitor the alcohol precipitation process of Reduning injection.
Chemical Precipitation ; Chromatography, High Pressure Liquid ; Drugs, Chinese Herbal ; chemistry ; Ethanol ; chemistry ; Lonicera ; chemistry ; Quality Control ; Spectroscopy, Near-Infrared ; methods

The present study was designed to determine the relationships between the performance of ethanol precipitation and seven process parameters in the ethanol precipitation process of Re Du Ning Injections, including concentrate density, concentrate temperature, ethanol content, flow rate and stir rate in the addition of ethanol, precipitation time, and precipitation temperature. Under the experimental and simulated production conditions, a series of precipitated resultants were prepared by changing these variables one by one, and then examined by HPLC fingerprint analyses. Different from the traditional evaluation model based on single or a few constituents, the fingerprint data of every parameter fluctuation test was processed with Principal Component Analysis (PCA) to comprehensively assess the performance of ethanol precipitation. Our results showed that concentrate density, ethanol content, and precipitation time were the most important parameters that influence the recovery of active compounds in precipitation resultants. The present study would provide some reference for pharmaceutical scientists engaged in research on pharmaceutical process optimization and help pharmaceutical enterprises adapt a scientific and reasonable cost-effective approach to ensure the batch-to-batch quality consistency of the final products.
Chemical Precipitation ; Chromatography, High Pressure Liquid ; methods ; Drugs, Chinese Herbal ; analysis ; chemistry ; Ethanol ; Injections ; Principal Component Analysis