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

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

According to the effect of second ethanol precipitation (SEP) in the production of Danshen injection, the indicators for controlling the quality of a concentration process of the supernatant obtained in the first ethanol precipitation (FEP) were investigated. The concentrated supernatants of FEP with different constituents were prepared and treated with the same amount of ethanol. The parameters which affect phenolic compound retention ratios in SEP supernatant were found using a stepwise regression method. Phenolic compound contents in SEP supernatant were mainly affected by pH and caffeic acid content of the concentrated supernatant of FEP. Caffeic acid content and pH should be set as quality indicators and strictly controlled in concentrating the supernatant of FEP.
Caffeic Acids ; chemistry ; Chemical Precipitation ; Ethanol ; chemistry ; Hydrogen-Ion Concentration ; Injections ; Plant Extracts ; chemistry ; Quality Control ; Regression Analysis ; Salvia miltiorrhiza ; chemistry

A novel paper-based analytical device(PAD)was prepared and applied to determine the xanthine oxi-dase(XOD)inhibitory activity of Salvia miltiorrhiza extracts(SME).First,polycaprolactone was 3D printed on filter paper and heated to form hydrophobic barriers.Then the modified paper was cut according to the specific design.Necessary reagents including XOD for the colorimetric assay were immobilized on two separate pieces of paper.By simply adding phosphate buffer,the reaction was performed on the double-layer PAD.Quantitative results were obtained by analyzing the color intensity with the specialized device system(consisting of a smartphone,a detection box and sandwich plates).The 3D-printed detection box was small,with a size of 9.0 cm x 7.0 cm x 11.5 cm.Color component G performed well in terms of linearity and detection limits and thus was identified as the index.The reaction con-ditions were optimized using a definitive screening design.Moreover,a 10％glycerol solution was found to be a suitable stabilizer.When the stabilizer was added,the activity of XOD could be maintained for at least 15 days under 4℃or-20℃storage conditions.The inhibitory activity of SME was investigated and compared to that of allopurinol.The results obtained with the PAD showed agreement with those ob-tained with the microplate method.In conclusion,the proposed PAD method is simple,accurate and has a potential for point-of-care testing.It also holds promise for use in rapid quality testing of medicinal herbs,intermediate products,and preparations of traditional Chinese medicines.

Since 2016, a number of studies have been published on standard decoctions used in Chinese medicine. However, there is little research on statistical issues related to establishing the quality standards for standard decoctions. In view of the currently established quality standard methods for standard decoctions, an improvement scheme is proposed from a statistical perspective. This review explores the requirements for dry matter yield rate data and index component transfer data for the application of two methods specified in “Technical Requirements for Quality Control and Standard Establishment of Chinese Medicine Formula Granules,” which include the average value plus or minus three times the standard deviation (X-±3SD) or 70% to 130% of the average value (X-±30%X-). The square-root arcsine transformation method is used as an approach to solve the problem of unreasonable standard ranges of standard decoctions. This review also proposes the use of merged data to establish a standard. A method to judge whether multiple sets of standard decoction data can be merged is also provided. When multiple sets of data have a similar central tendency and a similar discrete tendency, they can be merged to establish a more reliable quality standard. Assuming that the dry matter yield rate and transfer rate conform to a binomial distribution, the number of batches of prepared slices that are needed to establish the standard decoction quality standard is estimated. It is recommended that no less than 30 batches of prepared slices should be used for the establishment of standard decoction quality standards.