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Objective:To prepare Danshen extract and Danshen capsules, and study on its stability under high humidity, high temperature and light conditions.To determine the hygroscopicity of Danshen capsules and its intermediates. Method:The contents of danshensu, rosmarinic acid, lithospermic acid and salvianolic acid B in Danshen extract and Danshen capsules were determined by UPLC, the detection wavelength was 280 nm and the mobile phase was 0.05% phosphoric acid aqueous solution(A)-acetonitrile(B)for gradient elution(0-2 min, 93% -79.2% A;2-6 min, 79.2% -75% A;6-9 min, 75% -65% A;9-10.5 min, 65% -10% A;10.5-11 min, 10% -93% A).The critical relative humidity(CRH) was calculated and hygroscopic isothermal curve was drawn by determining the moisture absorption and weight gain of Danshen capsules and its intermediates. Result:The fluctuation of contents of these four phenolic acids in Danshen extract and Danshen capsules was within±10% and no significant change trend after placing at temperature of 40℃, relative humidity of 75% and 92.5%, light intensity of (4 500±500) Lx for 10 days.The change rates of danshensu in Danshen extract and Danshen capsules under 60℃ were 47.45% and 32.24%, and change rates of salvianolic acid B were -6.39% and -9.64%, respectively.The hygroscopic investigation showed that CRH of starch-based pellets was 58.5%, CRH of Danshen extract was 72.34%, CRH of coated pills was 72.85%, and CRH of Danshen capsules was 73.55%. Conclusion:High temperature has effect on stability of phenolic acids in Danshen extract and Danshen capsules, in order to ensure the quality of them, high temperature environment should be avoided.In order to prevent excessive moisture absorption of Danshen capsules and its intermediates, the relative humidity in the production and storage environment should be controlled below the corresponding CRH.
ABSTRACT
To establish an on-line monitoring method for extraction process of Schisandrae Chinensis Fructus, the formula medicinal material of Yiqi Fumai lyophilized injection by combining near infrared spectroscopy with multi-variable data analysis technology. The multivariate statistical process control (MSPC) model was established based on 5 normal batches in production and 2 test batches were monitored by PC scores, DModX and Hotelling T2 control charts. The results showed that MSPC model had a good monitoring ability for the extraction process. The application of the MSPC model to actual production process could effectively achieve on-line monitoring for extraction process of Schisandrae Chinensis Fructus, and can reflect the change of material properties in the production process in real time. This established process monitoring method could provide reference for the application of process analysis technology in the process quality control of traditional Chinese medicine injections.
ABSTRACT
Currently, near infrared spectroscopy (NIRS) has been considered as an efficient tool for achieving process analytical technology(PAT) in the manufacture of traditional Chinese medicine (TCM) products. In this article, the NIRS based process analytical system for the production of salvianolic acid for injection was introduced. The design of the process analytical system was described in detail, including the selection of monitored processes and testing mode, and potential risks that should be avoided. Moreover, the development of relative technologies was also presented, which contained the establishment of the monitoring methods for the elution of polyamide resin and macroporous resin chromatography processes, as well as the rapid analysis method for finished products. Based on author's experience of research and work, several issues in the application of NIRS to the process monitoring and control in TCM production were then raised, and some potential solutions were also discussed. The issues include building the technical team for process analytical system, the design of the process analytical system in the manufacture of TCM products, standardization of the NIRS-based analytical methods, and improving the management of process analytical system. Finally, the prospect for the application of NIRS in the TCM industry was put forward.
ABSTRACT
Growth year is one of the important factors for the quality of mountain cultivated ginseng (MCG). For age differentiation of MCG, rhizome extracts of ginseng aged from 11 to 15 years were analyzed using a non-targeted approach with ultra-performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS)-based on plant metabolomics technique. Multivariate statistical methods such as principal component analysis (PCA) and orthogonal partial least squared discrimination analysis (OPLS-DA) were used to compare the derived patterns among the samples. The results showed that the chemical constituents of MCG rhizome extracts of ginseng aged from 11 to 15 years were different. The data set was subsequently applied to metabolite selection by variable importance in the projection (VIP) for sophisticated classification with the optimal number of metabolites. The OPLS-DA model of MCG has a high interpretability and predictive capability, which established by selecting metabolites of MCG aged from 11 to 15 years. By this approach, MCG samples aged from 11 to 15 years, which are the most in demand in the Chinese ginseng market, can be precisely differentiated on the basis of selected metabolites. This proposed analytical method is fast, accurate, and reliable for discriminating the growth year of MCG. Moreover, this study supplies a new method for the age discrimination of other Chinese medicinal materials.
ABSTRACT
To study and establish a monitoring method for macroporous resin column chromatography process of salvianolic acids by using near infrared spectroscopy (NIR) as a process analytical technology (PAT).The multivariate statistical process control (MSPC) model was developed based on 7 normal operation batches, and 2 test batches (including one normal operation batch and one abnormal operation batch) were used to verify the monitoring performance of this model. The results showed that MSPC model had a good monitoring ability for the column chromatography process. Meanwhile, NIR quantitative calibration model was established for three key quality indexes (rosmarinic acid, lithospermic acid and salvianolic acid B) by using partial least squares (PLS) algorithm. The verification results demonstrated that this model had satisfactory prediction performance. The combined application of the above two models could effectively achieve real-time monitoring for macroporous resin column chromatography process of salvianolic acids, and can be used to conduct on-line analysis of key quality indexes. This established process monitoring method could provide reference for the development of process analytical technology for traditional Chinese medicines manufacturing.
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In present study, an ultra-performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UHPLC-QTOF/MS)-based plant metabolomics approach was established to investigate the metabolic profiles of the leaves, main root, branch root, and rhizome of Mountain Cultivated Ginseng (MCG). The UHPLC-QTOF/MS data were subjected to principal component analysis (PCA) and orthogonal partial least squared discrimination analysis (OPLS-DA) to find the potential characteristic components of the four parts of MCG in a quick way. The four different parts could be separated into four different groups of phytochemicals according to the PCA scores. The chemical constituents in four parts of MCG were obviously different. The identities of 81 major peaks that were detected in the four parts of MCG and the potential markers were identified by comparison with the reference compounds or were tentatively assigned by matching the retention time,empirical molecular formula and fragment ions with those of the published compounds of the Panax species. This proposed analytical method is fast, accurate, and reliable for differentiating the different parts of MCG. Moreover, this study supplied a new method for the quality evaluation of other Chinese medicinal materials.
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<p><b>OBJECTIVE</b>An UPLC method was developed to evaluate the quality of Paeoniae Radix by simultaneously determining four components, paeoniflorin, albiflorin, benzoylpaeoniflorin and paeonol in Paeoniae Radix Alba decoction pieces.</p><p><b>METHOD</b>The UPLC chromatographic column was ACQUITY UPLC® HSS T3. The mobile phase was acetonitrile-0.05% phosphoric acid water with gradient elution. The column temperature was 30 °C and detection wavelength was 230 nm with a flow rate of 0.4 mL · min(-1). A linear model was obtained through principal component analysis (PCA), and PCA scores were used to evaluate the quality of Radix Paeoniae Alba decoction pieces comprehensively.</p><p><b>RESULT</b>Paeoniflorin, albiflorin, benzoylpaeoniflorin and paeonol could be well separated from other components, and the results of specificity, precision, repeatability, linearity, recovery rate and stability reached the standards, respectively. The content of paeoniflorin in 9 batches of Paeoniae Radix Alba decoction pieces was below the standard given by Chinese Pharmacopoeia (2010 edition). Using the comprehensive scoring method with principal component analysis, the results showed that the samples from Zhejiang province have better quality than those from Anhui and Shandong provinces.</p><p><b>CONCLUSION</b>The method established in this study can effectively determine the content of paeoniflorin, albiflorin, benzoylpaeoniflorin and paeonol, which could be used for quality control of Paeoniae Radix Alba.</p>
Subject(s)
Drugs, Chinese Herbal , Paeonia , Chemistry , Principal Component AnalysisABSTRACT
After studying the discipline of chemical components distribution in peony root, it was found that the content distribution of albiflorin, paeoniflorin, benzoylpaeoniflorin and paeonol was inhomogeneous in different parts of peony root, as same as in different roots belonging to a same plant. Therefore, in order to minimize the effects of different qualities of materials on experimental result, the content changing percentages of four chemical components was chosen as indicators to study processing method of Paeoniae Radix Alba. The processing technique of Paeoniae Radix Alba was put peony roots in the boiled water for at most ten minutes, and cut them into 2-3 mm slices after peeling the root bark, finally dry them in a oven under 55 degrees C, which was similar to the traditional processing method used in Bozhou. And the peeling, boiling and drying methods would affect the contents of albiflorin, paeoniflorin, benzoylpaeoniflorin and paeonol on several levels.
Subject(s)
Chemistry, Pharmaceutical , Methods , Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Chemistry , Paeonia , Chemistry , Plant Roots , ChemistryABSTRACT
To ensure the stability of chemistry components and the convenience of operation, ultrasound method was chosen to study in this investigation. As the total common peaks area in chromatograms was set to be evaluation index, the influence on the technology caused by extraction time, ethanol concentration and liquid-to-solid ratio was studied by using single factor methodology, and the extraction technology of Paeoniae Radix Alba was optimized by using response surface methodology. The results showed that the extracting results were most affected by ethanol concentration; liquid-to-solid ratio came the second and extraction time thirdly. The optimum ultrasonic-assisted extraction conditions were as follow: the ultrasonic extraction time was 20.06 min, the ethanol concentration in solvent was 72.04%, and the liquid-to-solid ratio was 53.38 mL · g(-1), the predicted value of total common peaks area was 2.1608 x 10(8). Under the extraction conditions after optimization, the total common peaks area was 2.1422 x 10(8), and the relative deviation between the measured and predicted value was 0.86%, so the optimized extraction technology for Paeoniae Radix Alba is suitable and feasible. Besides, for the purpose of extracting more sufficiently and completely, the optimized extraction technology had more advantages than the extraction method recorded in the monogragh of Paeoniae Radix Alba in Chinese Pharmacopoeia, which will come true the assessment and utilization comprehensively.
Subject(s)
Paeonia , Chemistry , Technology, Pharmaceutical , MethodsABSTRACT
The ginsenoside-Ro is sensitive to be hydrolyzed in an alkaline medium. This paper investigated the hydrolysis kinetics of ginsenoside-Ro under different pH and temperature values. The results showed ginsenoside-Ro in alkaline solution followed pseudo-first-order reaction. Hydrolysis kinetics of ginsenoside-Ro has not been reported previously. The hydrolysis rate was independent of initial concentration. On the basis of UFLC-MS/MS, NMR, as well as chemical evidence,the structure of hydrolyzate was assigned as 3-O- [beta-D-glucuronopyranosyl- (1 --> 2) -beta-D-glucopyranosyl] -oleanolic acid.
Subject(s)
Drugs, Chinese Herbal , Chemistry , Ginsenosides , Chemistry , Hydrogen-Ion Concentration , Hydrolysis , Kinetics , Magnetic Resonance Spectroscopy , Mass Spectrometry , Molecular Structure , Spectrometry, Mass, Electrospray IonizationABSTRACT
<p><b>OBJECTIVE</b>To study the influence of different drying methods on the quality of Schisandrae Chinensis Fructus and thus provide useful reference for its proper drying methods.</p><p><b>METHOD</b>Schisandrae Chinensis Fructus was processed by eight drying methods including vacuum freeze drying, natural drying in the shade, drying in the sun, oven drying and vacuum drying under different temperature. The contents of the functional ingredients includes chisandrin, gomisin D, gomisin J, schisandrol B, angeloylgomisin H, angeloylgomisin Q, gomisin G, schisantherin A, deoxyschisandrin, schisandrin B, schisandrin C, 5-HMF, total aids and total sugars. The main components change after drying were analyzed by HPLC, ultraviolet spectrophotometry and potentiometric titration. Principal component analysis (PCA) was carried out by SPSS software to evaluate the quality of different processed products from Schisandrae Chinensis Fructus.</p><p><b>RESULT</b>All these results are in accordance with the requirements of Chinese Pharmacopoeia published in 2010, the contents of schisandrin and total eleven lignans were the highest using vacuum drying, and 5-HMF were the lower, oven drying made little difference but with lower schisandrin and higher 5-HMF as the heat increased.</p><p><b>CONCLUSION</b>Different drying methods have significant influence on the quality of Schisandrae Chinensis Fructus. Oven drying under 5°C should be adopted to substitute drying in the sun according to the China Pharmacopoeia published in 2010 for Schisandrae Chinensis Fructus by comprehensive analysis of the cost, content and practicality.</p>
Subject(s)
Desiccation , Methods , Drugs, Chinese Herbal , Chemistry , Quality Control , Schisandra , Chemistry , TemperatureABSTRACT
<p><b>OBJECTIVE</b>To compare the quality of red ginseng in different transplanting systems, and thus provide the basis for ginseng cultivation and processing.</p><p><b>METHOD</b>Based on the Chinese Pharmacopoeia and literature relating to red ginseng, the ten ginsenosides, total ash, acid-insoluble ash, volatile oil, ether extract and total protein of red ginseng in different transplanting systems were studied or determined.</p><p><b>RESULT AND CONCLUSION</b>The content of total ash and acid-insoluble ash in red ginseng was less than 5.0%, 0.3%, respectively. The content of three ginsenosides (Rg1, Re, Rb1) was in accordance with the requirements of Chinese Pharmacopoeia version 2010, and the content of ten ginsenosides was significant different.</p>