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.

Study on endpoint determination method of tablet coating based on 3σ criteria and logic regression / 中国中药杂志

This paper explores the statistical distribution characteristics of coating film thickness, so as to present a new method for determining coating endpoint based on 3σ criterion and logic regression. Firstly, the spectrum and thickness of 4 batch samples were collected. Secondly, the spectral range of normal products was obtained by 3σ criterion, with the spectral feature NI as the number of test spectrum in the above range. Then, the model based on 3σ criterion and logic regression was built according to the best condition in K-fold cross-validation and the determined threshold of qualified rate in the coating endpoint. Finally, the qualified rate of test set samples at different time points was calculated by the above model, and the above change trend and the threshold value were combined to determine the coating endpoint. The results of KS analysis showed the distribution of thickness of the qualified products followed the normal distribution(P=0.081>0.05). The accuracy of the coating endpoint determination was as high as 100% by the model based on 3σ criterion and logic regression when the determined threshold of qualified rate was 90%. Therefore, the 3σ criterion was feasible to the research of coating eligibility. This paper reveals certain random phenomena in the coating process, and the method features a high accuracy, quick analysis and a good interpretability, which provides a reference for online detection and qualify evaluation in future.

Research progress in the application of glass transition phenomenon in pharmaceutics / 药学学报

In recent years, the phenomenon of glass transition has been gradually applied to the field of pharmaceutics. And it exhibits important influences on multiple operating units of pharmaceutical preparations, and the properties and storage of pharmaceutical intermediates and products. At present, it has been widely used in the process of preparations such as drying, granulation, coating, tableting, holt-melt extrusion, cryogenic comminution, and so on. Meanwhile, it showed guiding significance for the process of preparation intermediates and their products, such as solid dispersion, microcapsule, liposome, particle, tablet, and other preparation intermediates and their products. Therefore, this article conducts a detailed analysis and systematic summary of the application guidance of the phenomenon of glass transition in the preparation process, and its influence on the preparation intermediates and products, so as to provide theoretical guidance for preparation production and product storage.

Analysis of Water Adsorption and Thermodynamic Properties of Three Rhei Radix et Rhizoma Decoction Pieces / 中国实验方剂学杂志

Objective:To investigate the moisture adsorption and thermodynamic characteristics of raw products， wine-processed products and fried charcoal products of Rhei Radix et Rhizoma， in order to guide their drying and storage. Method:Static isotherm weighing method was used to determine the adsorption isotherm curves of three Rhei Radix et Rhizoma decoction pieces at 25， 35， 45 ℃， and the test data were fitted with 7 commonly used water adsorption models to determine the best model for studying the adsorption thermodynamic parameters of these decoction pieces. Result:The best adsorption models of these three decoction pieces were all GAB model. At 25， 35， 45 ℃， the absolute safe moisture content of fried charcoal products was 7.43%， 6.79% and 6.20%， of wine-processed products was 8.68%， 8.17% and 7.03%， of raw products was 9.88%， 9.36% and 7.77%， respectively. At 25， 35， 45 ℃， the relative safe moisture content of fried charcoal products was 9.46%， 8.63% and 8.21%， of wine-processed products was 11.49%， 11.03% and 9.74%， of raw products was 13.49%， 12.66% and 11.14%， respectively. The net equivalent heat of adsorption （Qst） and differential entropy （Sd） of these three kinds of decoction pieces all decreased with the increase of equilibrium moisture content， Qst and Sd were in accordance with the entropy-enthalpy complementary theory. The constant velocity temperatures of raw products， wine-processed products and fried charcoal products of Rhei Radix et Rhizoma were 386.66， 391.15， 394.34 K （unit conversion of 1 K=-272.15 ℃）， their Gibbs free energies were 0.372 2， 0.406 0， 0.372 2 kJ·mol-1， respectively. Their adsorption processes were an unspontaneous process driven by enthalpy. Conclusion:The orders of equilibrium moisture content， monomolecular layer moisture content， Qst and Sd of three Rhei Radix et Rhizoma decoction pieces are all raw products>wine-processed products>fried charcoal products. The moisture absorption capacity of the decoction pieces is ranked as raw products>wine-processed products>fried charcoal products. The frying and roasting process significantly affects the hygroscopicity and thermodynamic properties of the three decoction pieces， the reason for this difference may be that the high temperature of the stir-frying results in the decrease of the hygroscopic groups and the increase of the hydrophobic materials in raw products， and the change in the texture of the decoction pieces. The research on the water adsorption characteristics of three Rhei Radix et Rhizoma decoction pieces can provide reference for selecting their storage conditions and drying process.

Investigation of Decoction Process of Digda-4 Decoction / 中国实验方剂学杂志

Objective:To optimize the decoction process of Digda-4 decoction(DGD-4D), and provide reference for the standardization study of decoction of Mongolian medicine decoction. Method:Taking DGD-4D as model drug, different decoction methods of Mongolian medicine were compared, HPLC was used to determine contents of aesculetin, geniposide, picroside Ⅰ and picroside Ⅱ.On the basis of single factor tests, central composite design-response surface methodology was adopted to optimize the decoction process of DGD-4D with transfer rates of 4 components and dry extract rate as indexes, regression model fitting was carried out by Design-Expert 8.0.6 software, prediction model of process parameters was established, and the optimal process was verified. Result:The optimal decoction condition of DGD-4D was determined to be adding 40 times the amount of water and decocting for 17 min, decocting once.Transfer rates of aesculetin, geniposide, picroside Ⅰ, picroside Ⅱ and dry extract rate were 70.01%, 94.11%, 61.23%, 92.32%, 32.89%, respectively. Conclusion:The optimum decoction process of DGD-4D is established, it has important reference significance for excavating, sorting, improving the level of Mongolian medicine preparations and ensuring the consistency of their clinical efficacy.

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.

Glass transition of Chinese medicine extract powder and its application / 中国中药杂志

Glass transition theory is an important theory in polymer science, which is used to characterize the physical properties. It refers to the transition of amorphous polymer from the glassy state to the rubber state due to heating or the transition from rubber state to glassy state due to cooling. In this paper, the glassy state and glass transition of food and the similar relationship between the composition of Chinese medicine extract powder and food ingredients were described; the determination method for glass transition temperature (Tg) of Chinese medicine extract powder was established and its main influencing factors were analyzed. Meanwhile, the problems in drying process, granulation process and Chinese medicine extract powder and solid preparation storage were analyzed and investigated based on Tg, and then the control strategy was put forward to provide guidance for the research and production of Chinese medicine solid preparation.

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 different DE values of malto-dextrin on properties for Schisandrae Chinensis Fructus spray-dried powder / 中国中药杂志

The purpose of this study was to compare the effect of different DE values of malto-dextrin on Schisandrae Chinensis Fructus spray-dried powder. The glass transition temperature (Tg) of the spray-dried powder, powder properties and microscopic morphology were determined, and then the moisture absorption isotherms and the glass transition temperature were used to predict its storage stability. The study showed that after adding malto-dextrin, the powder rate was increased; moisture content was decreased; Tg was increased; mobility got better; produced spherical microstructure; and Tg was increased with the decrease of DE value. The water activity-equilibrium moisture content (aw-EMC) relationship in GAB models showed, the moisture absorption of powder was increased with the rising of DE value; and the equilibrium moisture content-glass transition temperature (EMC-Tg) relationship in Gordon-Taylor models showed that, Tg was decreased with the increase of moisture content. As a result, the storage critical condition of the spray-dried powder was improved, and along with the decrease of DE value, the critical water activity and the critical water content were increased. Therefore, the smaller the DE value, the greater the stability of the spray-dried powder.

Preparation and in vivo and in vitro evaluation of Pulsatilla Saponin D Solid Dispersions / 中草药

Objective: To prepare the solid dispersion of Pulsatilla saponin D (PSD-SD) and evalution its in vivo and in vitro drug release behavior. Methods: The PSD-SD was prepared by solvent method. Three carriers were used in the PSD-SD. Infrared spectroscopy (IR), differential thermal analysis (DSC), and X-ray diffraction (XRD) were used to determine the PSD-SD. Dissolution rates and pharmacokinetic parameters were evaluated in vitro and in vivo characteristics of the PSD-SD. Results: When the PEG 6000 was used as carrier, the solubility of PSD was increased from 2.39 to 7.06 mg/mL, and the cumulative release rate of PSD reached 90% in 60 min, and the bioavailability of PSD was increased to 2.24 times. Conclusion: The solid dispersion prepared PSD can increase the solubility, dissolution rate, and bioavailability.

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>

Study on in situ intestinal absorption of Pulsatilla saponin D in rats / 中草药

Objective: To investigate the intestinal absorption characteristics of Pulsatilla saponin D in rats. Methods: In situ single-pass intestinal perfusion model was used to inspect the absorption of Pulsatilla saponin D in the intestinal tract of rats. HPLC was used to determine the concentration of Pulsatilla saponin D in intestinal perfusion fluid samples. Absorption rate constant (Ka) and apparent permeability coefficient (Papp) were used as indexes to investigate the effects of absorption sites, drug concentration, different pH values, and P-glycoprotein (P-gp) inhibitor on Pulsatilla saponin D absorption. Results: There was the significant difference (Pileum>jejunum>duodenum. With the pH value increasing, the Ka and Papp values also increased and both of them had significant differences (P0.05); There was significant difference (P<0.05) in Ka and Papp values with and without P-gp inhibitor. Conclusion: Pulsatilla saponin D could be well absorbed in whole intestinal segments of rats, and the best intestinal absorption site is colon; The drug concentration in a certain range has no effect on Ka and Papp values, which preliminarily comfirms that the obsorption mechanism of Pulsatilla saponin D could be passive diffusion; Pulsatilla saponin D may be a substrate of P-gp and possess the saturation phenomenon of transporters.

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>

Review of effervescent technique in pharmaceutics research / 中国中药杂志

Effervescent technique, which can accelerate drug disintegration and dissolution, is usually applied in quick release preparations. Along with the development of pharmaceutical technique and theory, effervescent technique is used more and more extensively to adjust the behavior of drug release, such as in sustained and controlled release preparations, pulsatile drug delivery systems, and so on. This review demonstrated the new applying of effervescent technique in effervescent tablets, stomach floating forms, osmotic pump tablets and pulsatile drug delivery systems, adding to the critical common technique of effervescent forms in drug research. This will be benefit for the further research and development of effervescent technique.