Water migration and kinetics of Arecae Semen during moistening process / 中国中药杂志

In this study, low-field nuclear magnetic resonance(LF-NMR) and magnetic resonance imaging(MRI) were employed to analyze the water distribution, status, and migration in the moistening process of Arecae Semen. Peleg model was adopted to study the water absorption kinetics of Arecae Semen moistened at different water temperatures(10, 30, and 50 ℃). The Arecae Semen samples soaked at different water temperatures all contained four water states: binding water T_(21), non-flowing water T_(22), free water T_(23), and unbound water T_(24). Non-flowing water had the largest increase in peak area during the moistening process, followed by free water. The peak areas of non-flowing water, free water, and total water were correlated with the water content(P<0.01). Therefore, LF-NMR can quickly and non-destructively predict the water content of Arecae Semen during moistening. The peak area of non-flowing water and the content of free water were correlated with the content of arecoline in the soaking solution(P<0.01), which indicated that the faster flow of non-flowing water and more free water corresponded to more arecoline dissolved. The MRI images showed that the water migration pathway varied at different soaking temperatures, and the moistening degree obtained by this means was consistent with that obtained based on traditional experience. The rate constant K_1 fitted by Peleg model decreased with the increase in water temperature, while the capacity constant K_2 showed an opposite trend. The Arrhenius equation fitting of K_1 with temperature showed that the activation energy of Arecae Semen in the moistening process was 32.98 kJ·mol~(-1). LF-NMR/MRI can be used to analyze the water status and content and determine the end moisturing point of Arecae Semen. Peleg model can accurately describe the water absorption properties of Arecae Semen in the moistening process. The findings of this study can guide the moistening optimization and mechanism research of other seed Chinese medicinal materials.

[Correlation between water state and texture during moistening of Paeoniae Radix Alba by LF-NMR/MRI].

The changes of active ingredients content, moisture status and texture characteristics during the moistening of Paeoniae Radix Alba were studied by low-field NMR and imaging(LF-NMR/MRI) and texture analyzer, so as to analyze the correlation between LF-NMR parameters, texture characteristics and active ingredient content of Paeoniae Radix Alba during the moistening at diffe-rent times. The results showed that MRI technology could directly, vividly and accurately characterize the degree of moistening and the process of water migration, and the degree of moistening was consistent with the judgment results of traditional experience. The characteristics of moisture migration and moisture phase state in the moistening process of Paeoniae Radix Alba were that the total water content increased and existed in the form of free water, with an increased moisture mobility. In the case of dampening, the total water content did not increase, but the more watery part of the medicinal material was distributed to the less watery part, with a reduced fluidity. Finally, the medicinal materials were moistened, which can be mutually verified with the MRI results. The free water content and the total water content of Paeoniae Radix Alba had extremely negative correlations with hardness, surface toughness, internal toughness, Paeoniflorin and albiflorin contents(P<0.01). It showed that the use of LF-NMR/MRI and texture analyzer could better characterize the moistening process. It provides data characterization for the scientific connotation of "less soaking and more moisturizing, and the drug is completely saturated with water", and the traditional experience of "observing the water head". The feasible and objective evaluation method was helpful to optimize the softening process parameters, scientifically standardize the operating specifications, define the scienti-fic connotation of traditional Chinese medicine softening, and promote the inheritance and innovation of traditional Chinese medicine processing.

[Study on endpoint determination and process analysis of tablet coating based on near infrared spectroscopy].

To conduct endpoint determination of tablet coating and analyze coating process by near-infrared spectroscopy(NIRS). Firstly, the layered k-fold cross validation was used to discuss the optimal combination of spectral interval and preprocessing method, and the optimal result was used as the modeling condition. Secondly, in above condition, the qualitative model was proposed based on the throught of principal component analysis(PCA) and confidence interval, this model and the conformity test model were established respectively in this study, and the discrimination performance of coating eligibility was calculated. Then, the internal cross validation was used to obtain the coating end-point conforming rate as the threshold for determining the endpoint of tablet coating. Finally, the results of predicted conforming rate and discrimination parameters for the test samples of different batches were calculated with the above models, which were then further used for end-point detection and process analysis. As compared with the conformity test, this method proposed in this study was more accurate and stable in determining the coating conformity, and the coating endpoint can be accurately determined when 95% of the eligibility rate was used as the discriminant threshold. Meanwhile, in the process analysis, the change trend of the process parameters(model discrimination parameters, prediction conforming rate) was basically consistent with that in the conformity test. The results indicate that the method proposed in this study has a good and stable performance, which can be used to determine the endpoint of coating and analyze the process. It is of great significance to reduce the difference between batches and improve the product consistency. Meanwhile, this research method also lays a foundation for the future researches by online near infrared measurements.

Research on extraction process of Digeda-4 flavored decoction based on QbD concept / 中国中药杂志

To establish and validate the design space of the Digeda-4 flavored decoction( DGD-4D) extraction process by using the quality by design( Qb D) concept. With DGD-4D decoction pieces as a model drug,with the transfer rate of aesculin,picroside I,picroside Ⅱ,geniposide and the yield of extract as critical quality attributes( CQAs),the single factor experiment design was used to determine the level of each factor; the Plackett-Burman experiment design was used to select the critical process parameters( CPPs);and the Box-Behnken experiment design was used to optimize the extraction process. The design space of the DGD-4D extraction process was established,and finally,four experimental points were selected to verify the established model. The single factor experiment determined the levels of each factor,including soaking time 60 min and 30 min,water adding volume 12 times and 8 times,extraction time 90 min and 30 min,number of extraction times 3 times and 1 time,as well as extraction temperature 100 ℃ and 90 ℃.By Plackett-Burman experimental design,the DGD-4D water addition,extraction time and number of extraction times were determined to be CPPs. The Box-Behnken experimental variance analysis showed that P of the regression model was less than 0. 01 and the misstated value was more than 0. 01,indicating that the model had good predictive ability,and the operation space of CPPs in the DGD-4D extraction process was determined as follows: the amount of water addition was 10-12 times; extraction time 50-80 min; and number of extraction times was 3 times. The design space of DGD-4D extraction process based on the concept of Qb D is conducive to improving the stability of product quality and laying a foundation for the future development of DGD-4D.

Fingerprinting and multi-indicator quantitative analysis of Mongolian drug Digeda-4 decoction / 中国中药杂志

To establish the high performance liquid chromatography (HPLC) fingerprint for Digeda-4 decoction (DGD-4D), determine the contents of aesculetin, geniposide, picroside Ⅰ, picroside Ⅱ and ellagicacid in DGD-4D, and provide the scientific foundation for quality control of DGD-4D. The analysis was performed on Diamonsil(2) C₁₈ (4.6 mm×250 mm,5 μm) column, with methanol-0.1% phosphoric acid aqueous solution as mobile phase for gradient elution. The flow rate was 1.0 mL·min⁻¹; injection size was 10 μL; temperature was maintained at 30 °C, and the detection wavelength was set at 254 nm. The common mode of DGD-4D HPLC fingerprint was established, and the hidden information was analyzed by Chemometrics. Chromatographic peaks for DGD-4D were identified by HPLC and quantitative analysis was conducted for characteristic peaks. There were 17 common peaks in the fingerprints and the similarity of the fingerprints was over 0.9 in all 15 batches. The samples were broadly divided into four kinds by principal component analysis and clustering analysis. Four marker compounds were verified by partial least squares discriminant analysis, and No. 9, 12 and 14 peaks were identified as geniposide, picroside Ⅱ, and picroside Ⅰ respectively. The average recoveries were in the range of 95.91%-97.31%. The HPLC fingerprint method for content determination is reliable, accurate, rapid, simple, and reproducible, and can be used as one of the effective methods to control the quality of DGD-4D.

Isothermal adsorption, desorptionand thermodynamic properties of Scutellaria baicalensis pieces / 中国中药杂志

To study the characteristics of adsorption and desorption of Scutellaria baicalensis pieces. On the basic thermodynamic theory, thestatic method was adopted to obtain S. baicalensis pieces' isothermal adsorption and desorption data at 25, 35, 45 ℃, with the water activity between 0.10 and 0.85. Eight moisture models were selected to fit the data and then evaluated to determine the thermodynamic properties of S. baicalensis pieces. The results show that, among the eight adsorption models, Peleg fit the best, in which absolutely-safe and the relatively-safe moisture contents of S. baicalensis pieces were around 9.22% and 13.51% respectively; the net equivalent heat adsorption and desorption and the differential entropy of S. baicalensis pieces were closely related to moisture content, and decrease within crease of water content; when drying the pieces, 12.0% of moisture content can be taken as the drying end; both of adsorption and desorption processes were driven by enthalpy and non-spontaneous. The study on S. baicalensis pieces' isothermal adsorption and desorption rules can help advance studies on adsorption and desorption rules of Chinese herbal pieces, and play a good guiding role in optimizing storage conditions and drying process of Chinese herbal pieces.

Thermodynamic analysis of water adsorption and desorption process of Chinese herbal decoction pieces / 中国中药杂志

Based on the basic theory of thermodynamics, the thermodynamic parameters and related equations in the process of water adsorption and desorption of Chinese herbal decoction pieces were established, and their water absorption and desorption characteristics were analyzed. The physical significance of the thermodynamic parameters, such as differential adsorption enthalpy, differential adsorption entropy, integral adsorption enthalpy, integral adsorption entropy and the free energy of adsorption, were discussed in this paper to provide theoretical basis for the research on the water adsorption and desorption mechanism, optimum drying process parameters, storage conditions and packaging methods of Chinese herbal decoction pieces.

Effect of air humidity on traditional Chinese medicine extract of spray drying process and prediction of its powder stability / 中国中药杂志

In order to solve the adhesion and the softening problems of traditional Chinese medicine extract during spray drying, a new method of adding dehumidified air into spray drying process was proposed, and the storage stability conditions of extract powder could be predicted. Kouyanqing extract was taken as model drug to investigate on the wet air (RH = 70%) and dry air conditions of spray drying. Under the dry air condition, the influence of the spray drying result with different air compression ratio and the spray-dried powder properties (extract powder recovery rate, adhesion percentage, water content, angle of repose, compression ratio, particle size and distribution) with 100, 110, 120, 130, 140 °C inlet temperature were studied. The hygroscopic investigation and Tg value with different moisture content of ideal powder were determined. The water activity-equilibrium moisture content (aw-EMC) and the equilibrium moisture content-Tg (EMC-Tg) relationships were fitted by GAB equation and Gordon-Taylor model respectively, and the state diagram of kouyanqing powder was obtained to guide the rational storage conditions. The study found that in the condition of dry air, the extract powder water content decreased with the increase of air compression ratio and the spray drying effect with air compression ratio of 100% was the best performance; in the condition of wet air, the extract powder with high water content and low yield, and the value were 4.26% and 16.73 °C, while, in the dry air condition the values were 2.43% and 24.86 °C with the same other instru- ment parameters. From the analysis of kouyanqing powder state diagram, in order to keep the stability, the critical water content of 3.42% and the critical water content of 0.188. As the water decreased Tg value of extract powder is the major problem of causing adhesion and softening during spray drying, it is meaningful to aid dehumidified air during the process.

Determination of equilibrium solubility and n-octanol/water partition coefficient of pulchinenosiden D by HPLC / 中国中药杂志

<p><b>OBJECTIVE</b>To determine the equilibrium solubility of pulchinenosiden D in different solvents and its n-octanol/water partition coefficients.</p><p><b>METHOD</b>Combining shaking flask method and high performance liquid chromatography (HPLC) to detect the n-octanol/water partition coefficients of pulchinenosiden D, the equilibrium solubility of pulchinenosiden D in six organic solvents and different pH buffer solution were determined by HPLC analysis.</p><p><b>RESULT</b>n-Octanol/water partition coefficients of pulchinenosiden D in different pH were greater than zero, the equilibrium solubility of pulchinenosiden D was increased with increase the pH of the buffer solution. The maximum equilibrium solubility of pulchinenosiden D was 255.89 g x L(-1) in methanol, and minimum equilibrium solubility of pulchinenosiden D was 0.20 g x L(-1) in acetonitrile.</p><p><b>CONCLUSION</b>Under gastrointestinal physiological conditions, pulchinenosiden D exists in molecular state and it has good absorption but poor water-solubility, so increasing the dissolution rate of pulchinenosiden D may enhance its bioavailability.</p>

Roller compaction research of Banlangen effervsce tablets / 中国中药杂志

<p><b>OBJECTIVE</b>To study the conditions and parameters of roller compaction of Banlangen effervsce tablet.</p><p><b>METHOD</b>The experimentation adopts L9 (3(4)) orthogonal experiment to study the conditions and parameters of roller compaction of Banlangen effervsce tablet; studied factors that included roller pressure, roller speed and moisture content of power, which influence the result of granule yield and granule friability.</p><p><b>RESULT</b>The optimal technique is: roller pressure at 1.5 MPa; roller speed at 15 Hz; moisture content of power at 1.5%.</p><p><b>CONCLUSION</b>The study of roller compaction technique of Banlangen effervsce tablets provides some technicial consults of its research and production.</p>

Effects of Huoxiang Zhengqi liquid on enteric mucosal immune responses in mice with Bacillus dysenteriae and Salmonella typhimurium induced diarrhea / 中国中药杂志

<p><b>OBJECTIVE</b>To explore the effects of Huoxiang Zhengqi liquid (HXZQ) on enteric mucosal immune responses in mice with Bacillus dysenteriae and Salmonella typhimurium induced diarrhea (BSD).</p><p><b>METHOD</b>Mice were randomly divided into four groups with 10 mice in each group: control group (control), BSD group, Huoxiang Zhengqi liquid treated BSD groups at high dosage and low dosage (HXZQ high, HXZQ low). HXZQ was administrated from the day of diarrhea induction at dosage of 5.21 g kg(-1) and 0.52 g kg (-1) respectively. Peyer's patch and periphery lymphocytes were prepared for flow cytometry, and level of TNF-alpha in periphery and enteric tissue homogenate were determined with ELISA. Student's t-test was used for statistics.</p><p><b>RESULT</b>Mice in BSD group started showing continuous diarrhea at the day of induction till the fourth day when the mice were sacrificed. Diarrhea in the mice of HXZQ high and low groups lasted for 36 and 54 h respectively. There were more CD4+ and CD8+ cells in periphery, less CD4+ cells in peyer's patch in BSD mice comparing to normal mice. In peyer's patch, there were more CD8+ cells in mice in HXZQ high and low groups and more CD4+ in mice in HXZQ high group. Higher level TNF-alpha in periphery and intestinal tissue homogenate in BSD group were observed. Mice in HXZQ high group showed the decreased level TNF-alpha in periphery and enteric tissue homogenate.</p><p><b>CONCLUSION</b>The immune regulation on peyer's patch CD4+ and CD8+ cells and suppression on TNF-alpha level in enteric homogenate might partially explain the effect of HXZQ on improvement of BSD.</p>

Study on uniform-design for optimizing supercritical-CO2 fluid extraction technique of tanshinones in radix salviae / 中国中药杂志

<p><b>OBJECTIVE</b>To explore the optimal supercritical-CO2 fluid extraction technique of extracting tanshinones in Radix salviae.</p><p><b>METHOD</b>The contents of tanshinones were determined by HPLC. Choosing the overall contents of 3 tanshinones as inspecting marker and uniform-design as method, the experimentation was carried out to study the main factors that influence the result of extraction.</p><p><b>RESULT</b>Among all the 5 inspected factors, the amount of entrainer was most notable. The optimal technique of extraction was: extraction pressure at 30 MPa; extraction temperature at 40 degrees C; separation pressure of separating kettle I at 6 MPa; separation temperature of separating kettle I at 50 degrees C; the amount of entrainer at 10%.</p><p><b>CONCLUSION</b>Adopting supercritical-CO2 fluid extraction method to extract the tanshinones in Radix salviae was feasible. The contents of tanshinones in the extract were high and the manipulation was simple, convenient and time saving.</p>