Effect of Different Steaming Processes on Variation of Active Ingredients in Notoginseng Radix et Rhizoma / 中国实验方剂学杂志

ObjectiveTo study on the correlation between the apparent color， near-infrared spectroscopy and dynamic changes of index constituent content of samples during the processing of steamed Notoginseng Radix et Rhizoma， and to provide reference for the processing process optimization and quality control of this decoction piece. MethodSamples were dried and crushed by setting three steaming temperature gradients of 100-105， 114-118， 130-136 ℃， and sampled at steaming times of 1， 2， 4， 8， 12， 24 h， respectively. The effects of different steaming temperatures and times on the color and absorption of steamed Notoginseng Radix et Rhizoma at different infrared wavelengths were observed， and principal component analysis and cluster analysis were performed on the obtained data by R 4.1.0 and SPSS 21.0 software to observe the changes in color and infrared absorption characteristics of samples. High performance liquid chromatography （HPLC） was employed to determine the content changes of notoginsenoside R1， ginsenoside Rg1， ginsenoside Rb1， ginsenoside Re， 20（S）-ginsenoside Rg3 and 20（R）-ginsenoside Rg3 before and after steaming of Notoginseng Radix et Rhizoma， mobile phase was acetonitrile （A）-water （B） for gradient elution （0-30 min， 19%A； 30-60 min， 19%-44%A； 60-78 min， 44%-74%A； 78-80 min， 74%-100%A； 80-86 min， 100%A； 86-87 min， 100%-19%A； 87-95 min， 19%A） with the detection wavelength of 203 nm. ResultDuring the steaming process of Notoginseng Radix et Rhizoma， with the increase of steaming temperature and time， the b* （yellow-blue value）， L* （brightness）， △E* （comprehensive color difference value） of sample powder showed a decreasing trend， while the a* （red-green value） showed an increasing trend， and the color gradually deepened from gray to brown and dark black. There was no significant difference in the infrared absorption between raw and steamed Notoginseng Radix et Rhizoma sample powder in the low and medium wavelength bands， but significant difference in the infrared absorption of high band， especially in the band of 9 600-10 000 cm-1. HPLC showed that the contents of the original components （notoginsenoside R1， ginsenoside Rg1， Re and Rb1） decreased and 20（S）-ginsenoside Rg3 and 20（R）-ginsenoside Rg3 were newly produced after steaming of Notoginseng Radix et Rhizoma. The content proportion of these six index components reached the best when the steaming temperature at 130-136 ℃ and the steaming time of 1 h. ConclusionThe color and infrared absorption of samples are affected by the dynamic changes of chemical composition during the steaming process， and the composition change is the result of the joint influence of steaming temperature and time. In this paper， through multi-dimensional analysis of the apparent color indexes， the change pattern of near-infrared absorption characteristics and the index components of the samples， the different process parameters of steamed Notoginseng Radix et Rhizoma were evaluated holistically， and the quality transfer pattern of its processing process was initially revealed， which can provide scientific basis for processing optimization and quality evaluation of steamed Notoginseng Radix et Rhizoma.

Quality evaluation of Aralia taibaiensis based on spectrum-activity relationship / 中国中药杂志

A spectrum-activity relationship is established with high performance liquid chromatography(HPLC) fingerprints and the in vitro antioxidant activity to improve the quality evaluation system of Aralia taibaiensis. The HPLC profiles of 12 batches of samples were collected, and the similarity evaluation, heat map analysis and principal component analysis were conducted for the chemometric study of the fingerprint data. Combined with grey correlation analysis, the contributions of the common peaks in the fingerprints to the antioxidant activity were clarified, and the important peaks reflecting the efficacy were identified. The results showed that 17 common peaks were found in 12 batches of A. taibaiensis samples, and 6 of them were identified as saponins. Similarity evaluation, heat map analysis and principal component analysis roughly classified the A. taibaiensis herbs into two categories, i.e.,(1) S1-S10, S12 and(2) S11. Twelve batches of samples showed different antioxidant activities in a dose-dependent manner. In particular, S9 had the strongest antioxidant activity, while S11 was the weakest in antioxidant capacity, which was basically consistent with the overall score results. The results of grey correlation analysis demonstrated that the 17 common peaks scavenged DPPH radicals in the following order: X_3>X_(17)>X_4>X_8>X_7>X_(13)>X_2>X_6>X_(11)>X_(10)>X_(16)>X_(12)>X_9>X_5>X_(14)>X_1>X_(15), and scavenged ABTS radicals in the order of X_4>X_3>X_7>X_8>X_2>X_(17)>X_(13)>X_6>X_(16)>X_(11)>X_5>X_(12)>X_(10)>X_9>X_(14)>X_1>X_(15). Among them, X_3, X_4, X_7(araloside C), X_8 and X_(17) were the important peaks reflecting the efficacy of A. taibaiensis, which were basically consistent with those contained in the principal component 1. In this study, the correlation between the HPLC fingerprints of 12 batches of A. taibaiensis and its antioxidant activity provides a reference for the Q-marker screening and quality control of A. taibaiensis.

Powder modificationfor improving content uniformity of Ziyin Yiwei Capsules / 中国中药杂志

Based on the defects in powder properties of the contents of Ziyin Yiwei Capsules, this study screened out the main medicinal slice powders causing the poor powdery properties, and introduced the powder modification process to improve the powdery properties of these slice powders, the pharmaceutical properties of the capsule contents, and the content uniformity of Ziyin Yiwei Capsules, so as to provide a demonstration for the application of powder modification technology to the preparation of Chinese medicinal solid preparations. Through the investigation on the powder properties of the contents of Ziyin Yiwei Capsules, it was clarified that the pulverized particle size of the capsule contents had a good correlation with the pulverization time. According to the measurement results of the powder fluidity and wettability, the quality defects of the capsule contents were caused by the fine powders of Taraxaci Herba and Lungwortlike Herba. "Core-shell" composite particles were prepared from medicinal excipients magnesium stearate and fine powders of Taraxaci Herba and Lungwortlike Herba slices after ultra-fine pulverization to improve the powder properties of the problematic fine powders. Powder characterization data including fluidity and wettability were measured, followed by scanning electron microscopy(SEM) and infrared ray(IR) detection. It was determined that the optimal dosage of magnesium stearate was 2%, and the compositing time was 3 min. The composite particles were then used as content components of the Ziyin Yiwei Capsules. The powder characteristics between the original capsule and the modified composite capsule including the particle size, fluidity, wettability, uniformity of bulk density, and uniformity of chromatism as well as the content uniformity and in vitro dissolution were compared. The results showed that the powder characteristics and content uniformity of the prepared composite capsule were significantly improved, while the material basis of the preparation was not changed before and after modification. The preparation process was proved to be stable and feasible. The powder modification technology solved the pharmaceutical defects that were easy to appear in the preparation of traditional capsules, which has provided experimental evidence for the use of powder modification technology for improving the quality of Chinese medicinal solid preparations and promoting the secondary development and upgrading of traditional Chinese medicinal dosage forms such as capsules.

Particle design for improving content uniformity of Hewei Jiangni Capsules / 中国中药杂志

Targeting the poor powder characteristics of the contents in Hewei Jiangni Capsules, this study characterized the powder properties of the contents and employed particle design technique for improving the content quality. The content composite particles of Hewei Jiangni Capsules prepared by the particle design technique were evaluated by scanning electron microscopy(SEM), followed by infrared ray(IR), content uniformity, and in vitro dissolution detection. It was found that there was a good correlation between the crushed particle size of slices and the crushing time, and the calcined Haematitum was responsible for the poor content uniformity. After the fine powder of calcined Haematitum was super-finely ground for 8.5 min and those of the other contents in the capsule for 1 min, they were prepared into the composite particles, whose property characterizations were compared with those of the physical mixtures. The content uniformity of the prepared composite particles was significantly improved, and the preparation process was stable and reliable. The adoption of particle design technology to correct the poor uniformity of the physical mixture, solve the pharmaceutical defects of Hewei Jiangni Capsules, and improve the quality of prescriptions has provided important reference for the clinical application and development of Chinese medicinal preparations.

Particle design for improving taste and homogeneity of traditional Chinese medicinal powder: taking Zhuhuang Chuihou Powder as an example / 中国中药杂志

Due to the complex source and different physical and chemical properties of traditional Chinese medicines(TCM) powder, there are many common pharmaceutical problems in its preparation, such as large particle size difference, poor mixing uniformity, and poor compliance with oral intake, which has directly affected the quality of solid preparations as well as their clinical efficacy and safety. This study observed the property of Zhuhuang Chuihou Powder and extract its pharmaceutical defects. It was found that realgar and calcined Borax in Zhuhuang Chuihou Powder were heavy in texture and toxic, and they were easy to be isolated, indicating the potential safety hazard. At the same time, Coptidis Rhizoma and Phellodendri Chinensis Cortex were the main sources of its bitterness. Therefore, based on the idea of "drug-excipients unity", the particle design technology was used to prepare core/shell-type composite particles with bitter medicines as the core and mineral medicines as shell. Both infrared spectroscopy and scanning electron microscopy results indicated the formation of composite particles, and the taste of these composite particles were improved. Compared with the physical mixtures, the composite particles exhibited significantly decreased RSD values in the content uniformity of berberine hydrochloride, arsenic disulfide, and sodium tetraborate and appearance uniformity. The introduction of particle design technology solved the problem of uneven dispersion of Zhuhuang Chuihou Powder, thus ensuring its uniform dispersion, stability, and control and improving the quality of the original preparation. This has provided a scientific basis for the quality control of TCM powder.

Application of design technology for preparing Lingzhu Powder particles based on solvent evaporation method / 中国中药杂志

Targeting the deficiencies of Lingzhu Powder, this study introduced the particle design technology to improve its quality. Based on the mechanism of particle design for powder and the characteristics of solvent evaporation method, composite particles consisting of Succinum, Cinnabaris, and artificial Bovis Calculus were prepared. And the powder properties of composite particles and physical mixtures as well as the content uniformity of toxic components were investigated for exploring the technological advantages of particle design in improving the quality of Lingzhu Powder. The results showed that the composite particles prepared using solvent evaporation method and particle design technology were micro-particles, and the stable agglomerate structure could be observed under SEM. Composite particles exhibited better fluidity and compliance in oral intake than physical mixtures. The differences in chromatism, bulk density, and content uniformity of the composite particles were smaller than those of physical mixtures, and the corresponding RSD values \[4.8%, 1.8%, 3.4%(bilirubin), and 0.63%(HgS), respectively\] were smaller. The solvent evaporation combined with particle design technology can be utilized to significantly improve the quality of Lingzhu Powder, which has provided new ideas for the optimization of the quality of traditional Chinese medicinal powder.

Application of particle design technology in field of traditional Chinese medicine powder / 中国中药杂志

Solid preparations account for more than 50% of traditional Chinese medicines(TCM). TCM powder is an important raw material for solid preparations of TCM. Its powder properties directly affect the quality of solid preparations, and even clinical safety and effectiveness. Particle design technology based on the characteristics of powder in TCM is an important means to improve and enhance the quality of solid preparations. This study summarized the relevant principles, methods, characteristics, classification, equipment, and other elements of particle design technology in recent years, analyzed the difficulties in its application in the field of TCM powder, and proposed the strategies in conjunction with the development of computer data mining. The present study is expected to provide a reference for the suitability of particle design in the field of TCM powder.

Effect of Compound Longmaining on TLR4/MyD88/NF-κB p65 Signaling Pathway in Rats with Acute Myocardial Infarction / 中国实验方剂学杂志

Objective: To investigate the protective effect of compound Longmaining isoprenaline hydrochloride-induced myocardial infarction model and its effect on Toll-like receptor 4(TLR4)/myeloid differentiation factor 88(MyD88)/nuclear transcription factor-kappa B (NF-κB) signaling pathway.Method: Forty-eight male SD rats were randomly divided into 6 groups:normal group,model group,compound salvia miltiorrhiza drop pill group (0.072 9 g·kg-1),and low,medium and high-dose compound Longmaining decoction groups (0.36,0.71,1.43 g·kg-1).The acute myocardial infarction model was induced through subcutaneous injection with isoproterenol.The pathological changes of myocardial tissue were examined by hematoxylin-eosin (HE) staining.The levels of interleukin-1β(IL-1β),interleukin-6(IL-6),tumor necrosis factor-α(TNF-α),monocyte chemotaxis protein-1(MCP-1) and nitrogen (NO) in serum were measured by enzyme linked immunosorbent assay (ELISA).The expression levels of inhibitors of NF-κB kinase subunit-β(IKKβ),NF-κB inhibitor α(IκBα),TLR4,MyD88 and NF-κB p65 were measured by immunohistochemical staining and Western blot.Result: Compared with normal group,the myocardial injury in model group was obvious.The levels of IL-1β,IL-6,TNF-α,MCP-1 and NO in serum increased significantly (PκBα decreased significantly (Pβ,TLR4,MyD88 and NF-κB p65 increased significantly in myocardial tissue (Pβ,IL-6,TNF-α,MCP-1 and NO levels in the serum (PκBα(Pβ,TLR4,MyD88 and NF-κB p65(PConclusion: Compound Longmaining plays a protective effect on acute myocardial infarction by regulatingthe expressions of TLR4/MyD88/NF-κB p65 signaling pathway and relevant inflammatory factors.

Study on Stability of Volatile Oil in Foeniculi Fructus and Screening Its Antioxidants in Accelerated Oxidation Environment / 中国实验方剂学杂志

Objective: To screen the accelerated oxidation environment with the most drastic changes in the volatile oil composition of Foeniculi Fructus, and to optimize the type and concentration of antioxidants. Method: The volatile oil of Foeniculi Fructus was extracted by steam distillation. Taking thiobarbituric acid reactive substances (TBARS) value and peroxide value (POV) as evaluation indexes, response surface method was used to investigate the effects of temperature, concentrations of ferrous ion (Fe2+) and azoamidine initiator V50 (AAPH) on volatile oil components of Foeniculi Fructus and its oxidation products. TBARS and POV were detected by ultraviolet chromatography. The oxidative environment with the most drastic changes of volatile oil composition of Foeniculi Fructus was screened. The type and concentration of antioxidants were selected by single factor experiments. The change discipline of volatile oil in Foeniculi Fructus after added different concentrations of antioxidants were analyzed by GC-MS. Result: The worst oxidizing environment for volatile oil of Foeniculi Fructus was as follows:temperature at 42.5℃,AAPH concentration of 1 g·L-1,Fe2+ concentration of 20.85 mg·L-1. Ascorbyl palmitate with concentrations of 0.2 mol·L-1 and 0.8 mol·L-1 could effectively improve the stability of volatile oil from Foeniculi Fructus. Conclusion: Under the accelerated oxidation environment, the terpenes in volatile oil from Foeniculi Fructus are significantly changed, but its stability can be improved by ascorbyl palmitate.

The investigation of key factors influencing the extraction process of chuanxiong oil by steam distillation / 中国药学杂志

OBJECTIVE: To investigate the key process parameters that affect the extraction of essential oil from Ligusticum chuanxiong by steam distillation. METHODS: Volatile oil and emulsified aromatic water are the products of the extraction process of volatile oil. The nature of volatile oil will directly affect the formation of emulsified aromatic water. The influence of extraction temperature, the ratio of liquid to medicine, medicinal material granularity process parameters on the stability of the emulsified fragrance water and the yield of volatile oil were analyzed, furtherly the corresponding extraction process control model of volatile oil was established to reveal the key technology and parameter during the process of volatile oil extraction and separation. RESULTS: The relative viscosity, relative density, surface tension and contact angle of Ligusticum chuanxiong oil decreased gradually with the increase of temperature, while the interfacial tension increased with the increase of temperature. The liner model of aromatic water TSI and process parameters was TSI = 0. 877 + 0. 230 × extraction temperature - 0. 024 × comminution particle size + 0. 010 × liquid ratio + 0. 292 × condensation temperature + 0. 776 × collection temperature. The liner model of the physicochemical properties of TSI and volatile oil was TSI = 0. 877 - 0. 170 × density + 0. 098 × viscosity - 0. 301 × surface tension + 0. 695 × interfacial tension - 0. 060 × contact angle. The liner model of volatile oil yield and process parameters was that yield = 5. 065 + 0. 258 × extraction temperature + 0. 127 × particle size + 0. 016 × liquid ratio + 0. 264 × condensation temperature + 0. 264 × collection temperature + 0. 502 × TSI. The liner model with the physicochemical properties of volatile oil was the yield = 5. 065 - 0. 196 × density - 0. 167 × viscosity - 0. 201 × surface tension + 0. 153 × interfacial tension - 0. 065 × contact angle. CONCLUSION: TSI and yield of aromatic water of Ligusti-cum chuanxiong are directly proportional to the extraction temperature and comminution particle size of medicinal materials. The yield of volatile oil shows a significant positive correlation with the TSI value, which can reflect the yield of volatile oil and is a specific index that can evaluate the process parameters objectively.

Extraction kinetics of volatile oil from galangal by steam distillation / 中国中药杂志

To reveal the extraction regularity of volatile oil from galangal by GC-MS analysis. The volatile oil in galangal was extracted by steam distillation. The extract was collected every 30 min, the oil part and the water part were separated. GC-MS was used to analyze the extraction liquid collected at different time periods. A total of 140 volatile components were obtained by GC-MS analysis. Among them, the main components were eucalyptus oil alcohol, alpha-pine oil alcohol and 4-terpene alcohol; 22 special components were dissolved in water, 77 special components were dissolved in oil and 41 components were dissolved in both oil and water. With the increase of specific components in water, the content of Eucalyptus in water increased in a linear manner. The increase of eucalyptus oil further promoted the dissolution or dispersion of alpha PN in water, and the change of specific components in oil was positively correlated with the content of Eucalyptus and alpha-terpilenol in oil. The results of principal component analysis show that the physical and chemical properties of the compounds were important factors affecting the distribution of components. PC1 (molecular weight, melting point, boiling point positive correlation), PC2 (negative correlation of refractive index) and PC3 (positive correlation of water solubility) were the main components that lead to the differences in composition distribution. The process of extracting volatile oil from galangal through steam distillation was affected by the physical and chemical properties of volatile components. Some components were specifically distributed in the fragrance and volatile oil system. The endemic components of aromatic water increased the content of the main components in the water system, which may lead to the "emulsification", reduction of the yield and low quality of the volatile oil.

Extraction kinetics of volatile components from Foeniculum vulgare by steam distillation / 中草药

Objective To reveal the dissolution rule of volatile oil in the extraction processfrom Foeniculum vulgare by GC-MS analysis. Methods The volatile oil of F. vulgare was extracted by steam distillation; The volatile oil/perfume system was collected at fixed time interval (30 min); The volatile oil part and perfume part were separated. Using N-docosane and methyl myrisate as double internal standard, GC-MS was selected for analysis and quantification. The main components were extracted by thermography, and the distribution regularity of components was definited. The principal components with the impact on the composition distribution were investigated according to the physical and chemical properties of the molecular weight, melting point, boiling point, and density of the compounds. Results The GC-MS analysis results concluded 123 volatile components. The main components were estragole, anethole, and (R)-(+)-limonene. There were 60 and 27 endemic components in aromatic aqueous solution and volatile oil, respectively, in which 27were common composition. The content of anethole in water was positively related to the endemic components in aromatic water, and even had a positive correlation with anethole artemisia content and (R)-(+)-limonene content. The specific components in the oil were positively related to the content of the main components (R)-(+)-limonene in the volatile oil. The principal component analysis showed that the physical and chemical properties of the compounds were important factors affecting the distribution of components; PC1 (molecular weight and positive correlation of melting point), PC2 (refractive index positive correlation), and PC3 (water-soluble negative correlation) were the principal components that lead to differences in component distribution. Conclusion In the process of extracting volatile oil from F. vulgare, steam distillation is affected by the physical and chemical properties of volatile components. Some components are specifically distributed in aromatic perfume and volatile oil system. The endemic components of aromatic water increase the content of the main components in the water system, which may lead to theproduction of "emulsification" during the extraction process of volatile oil and reduce the yield and quality of volatile oil.