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Objective:To study the application of statistical process control technology to establish the real-time release criteria of alcohol precipitation process of ArtemisiaeAnnuae Herba and Lonicerae Flos. Methods: Twenty-ninebatches of samples came from alcohol precipitation process of ArtemisiaeAnnuae Herba and Lonicerae Flos were collected as the calibration set. The contents of neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, and solid content were determined to establish the quantitative real-timerelease criteria based on statistical process control technology. Thirteenbatches of alcohol precipitation process of ArtemisiaeAnnuae Herba and Lonicerae Flos were prepared under the different process conditions by the central composite design. They were regarded as the validation set to test the dependability of the real-time release criteria. Results: The established quantitative release ranges were neochlorogenic acid 0.279-0.541 mg/g, chlorogenic acid 1.941-2.610 mg/g, cryptochlorogenic acid 0.453-0.570 mg/g, and solid content3.565%-4.925%. The four index component contentsof the samples 1, 4, 8, 9, and 10 from the validation set werewithin the range of the real-time release criteria. Conclusion: Univariate statistical process control could be well monitored and understood of production process for Chinses materiamedica.They are used to achieve the purpose of real-time release.
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To evaluate the rationality of alcohol precipitation technology of Biqiu granule by investigating its effect on serum histamine, IgE, IL-4, IFN and TNF-α. The contents of cafferic acid and rosmarinic acid were used as the evaluation indexes, and some factors affecting index were firstly evaluated by Plackett-Burman design; then alcohol precipitation technology was further optimized by Box-Behnken design to determine the optimal alcohol precipitation conditions. The best alcohol precipitation conditions were as follows: the relative density of herb liquor was 1.15 (65 ℃); the concentration of alcohol was 70%, and standing time was 12 hours. Optimal alcohol precipitation technology of Biqiu granules determined by pharmacodynamic screening, Plackett-Burman and Box-Behnken design tests, was stable and feasible with good predictability, providing reliable basis for the industrialization production of Biqiu granules.
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To develop a method for the rapid monitoring of five components during the alcohol precipitation process of Shenzhiling oral solution using near infrared spectroscopy(NIRS).The contents of five components detemined by high performance liquid chromatography(HPLC) were used as the reference values, and the NIRS based partial least square regression(PLSR) models were used to monitor the concentrations of paeoniflorin, albiflorin, liquiritin, cinnamic acid and glycyrrhizic acid during the alcohol precipitation process of Shenzhiling oral solution, which were optimized and verified through comparing of different spectral pre-processing and variables selection methods. Determination coefficients(Rcal2 and Rpred2), root mean squares error of prediction (RMSEP), root mean squares error of calibration(RMSEC) and ratiao of performance to deviation(RPD) were applied to evaluate the performance of the models, and the corresponding values were 0.993 3 and 0.997 6, 0.084 9 g•L⁻¹, 0.073 3 g•L⁻¹ and 14.7 for paeoniforin; 0.991 4, 0.992 7, 0.028 1 g•L⁻¹, 0.030 5 g•L⁻¹ and 10.2 for albiforin; 0.955 3, 0.976 1, 0.012 0 g•L⁻¹, 0.012 3 g•L⁻¹ and 5.1 for liquiritin; 0.958 8, 0.990 3, 0.003 89 g•L⁻¹, 0.002 89 g•L⁻¹ and 7.1 for cinnamic acid; 0.982 0, 0.986 3, 0.053 8 g•L⁻¹, 0.059 0 g•L⁻¹, 7.2 for glycyrrhizic acid, respectively. The results indicated that the presented approach was effectively for the quantitative monitoring of the alcohol precipitation process of Shenzhiling oral solution.
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To optimize the alcohol precipitation process for Lonicerae Flos and Artemisiae Annuae Herba (LA) in Reduning Injection and obtain the relationship equation of the key process parameters and quality attributes, which could provided a theoretical basis of the control automization in the alcohol precipitation process. With the transfer rates of neochlorogenic acid, chlorogenic acid, cryptochlorogenin acid, caffeic acid, secoxyloganin and solid content in precipitation liquid as evaluation indexes, the effect of the seven factors, such as relative density and the temperature of LA in liquid phase before alcohol precipitation, alcohol concentration in the end of alcohol precipitation, stirring speed in alcohol precipitation, adding alcohol speed, standing temperature, and standing time, on the alcohol precipitation process was investigated by the single factor experiment. By analysis of variance, the key factors that could influence the alcohol precipitation process were determined. Then the range of parameters of key factors was further studied and explored by Box-Behnken response surface methodology. The optimum preparation conditions of the alcohol precipitation process of LA were as follows: stirring speed was 550 r/min, adding alcohol speed was 4.0 mL/s, standing temperature was 30℃, standing time was 24 h, alcohol concentration was 75%, the relative density of LA was 1.10, and the temperature of LA was 25℃. Under these conditions, the transfer rates of neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, and secoxyloganin were 94.8%, 97.6%, 97.4%, 97.2%, and 96.1%, and the solid content was 4.2%. The alcohol precipitation process of LA have been optimized by the response surface method, which could help to enhance the stability of the process.
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The data of the alcohol concentration in alcohol precipitation process of 22 Chinese materia medica (CMM) were investigated and analyzed. The result showed that the real alcohol concentration in the alcohol precipitation process was higher than the expected generally, and the real alcohol concentration in the alcohol precipitation process in the same product was different in different batches. The gap between the real alcohol concentration in the alcohol precipitation process and the expected maybe related to the product and the method to determine how much alcohol to be added and the way of operation. The data above were analyzed, and some suggestions were presented as follows: (1) Meaning of the expected alcohol concentration in the alcohol precipitation process described in the drug quality specification should be explained clearly; (2) The method used to determine how much alcohol should be added and the indicator of on-line control should be studied and determined; (3) During the process validation, the real alcohol concentration in the alcohol precipitation process should be detected according to the procedure in China Pharmacopeia (2010 edition) and make sure whether the real alcohol concentration in the alcohol precipitation process was the same as the expected; (4) The alcohol precipitation process of new CMM should be systematically studied, and the method used to determine how much alcohol should be added must be on record in `Production Process for Oon-site Inspection'.
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Objective: To investigate the preparation procedure of Zhenjing Xiehuo granules. Methods: Using the dry extract yielding rate and the contents of liquiritin and salvianolic acid B as the indices, an orthogonal test was adopted to choose the best ex-traction and purification technology. Using the qualified ratio of granules as the index, an orthogonal test was adopted to choose the best preparation process of the granules. Results:The optimized preparation conditions were as follows:Pulvis ferri was decocted first for 60 min. The other medicines were dipped in 8-fold amount of water for 90 min, and then added into pulvis ferri extracts and decocted for 3 times with 90 min for each time. The extracts were collected and concentrated till the relative density was 1. 3 (measured at 60℃), water was added with the dilution ratio of 1:2, ethanol was added till the percentage of ethanol was 50%, and then the mixed liquid was filtered after 24 hours. After ethanol was recycled from the filtrate, the filtrate was concentrated till the relative density was 1. 3 (measured at 60℃), and then dried at 60℃. Starch as the diluent, the ratio of extract to excipient was 1:0. 8, and the wet granules were prepared with 90% ethanol as the wetting agent, dried 3 hours at 60℃ followed by size stabilization to obtain the products. Con-clusion:The optimized preparation procedure of Zhenjing Xiehuo granules is stable and feasible.