1.Optimization of extraction technology for salidroside, tyrosol, crenulatin and gallic acid in Rhodiolae Crenulatae Radix et Rhizoma with orthogonal test.
Xin LUO ; Xue-jing WANG ; Yi-wu ZHAO ; Wen-zhe HUANG ; Zhen-zhong WANG ; Wei XIAO
China Journal of Chinese Materia Medica 2015;40(18):3590-3593
The extracting technology of salidroside, tyrosol, crenulatin and gallic acid from Rhodiolae Crenulatae Radix et Rhizoma was optimized. With extraction rate of salidroside, tyrosol, crenulatin and gallic acid as indexes, orthogonal test was used to evaluate effect of 4 factors on extracting technology, including concentration of solvent, the dosage of solvent, duration of extraction, and frequency of extraction. The results showed that, the best extracting technology was to extract in 70% alcohol with 8 times the weight of herbal medicine for 2 times, with 3 hours once. High extraction rate of salidroside, tyrosol, crenulatin and gallic acid were obtained with the present technology. The extracting technology was stable and feasible with high extraction rate of four compounds from Rhodiolae Crenulatae Radix et Rhizoma, it was suitable for industrial production.
Chemical Fractionation
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methods
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Chemistry, Pharmaceutical
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methods
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Coumarins
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isolation & purification
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Drugs, Chinese Herbal
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isolation & purification
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Gallic Acid
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isolation & purification
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Glucosides
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isolation & purification
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Phenols
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isolation & purification
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Phenylethyl Alcohol
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analogs & derivatives
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isolation & purification
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Rhizome
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chemistry
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Rhodiola
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chemistry
2.Fingerprint analysis of Resina Draconis from different manufactuers by UPLC coupled with chemometrics.
Jian-ping QIN ; Jia-chun LI ; Jian-xiong WU ; Su-su WU ; Wen-zhe HUANG ; Zhen-zhong WANG ; Wei XIAO
China Journal of Chinese Materia Medica 2015;40(6):1114-1118
This study is to establish an UPLC fingerprint of Resina Draconis from different manufacturers, which can provide a comprehensive evaluation for its quality control. The analysis was performed on a Phenomenex Kinetex 2.6 μ C18 100A column by agradientelution program with acetonitrile-water as mobile phase at a flow rate of 1.7 mL x min(-1). The column temperature was 40 degrees C and the detection wavelengthwas 280 nm. The fingerprints of 18 batches of Draconis Resina were further evaluated by chemometrics methods including similarity analysis (SA), hierarchical clustering analysis (HCA) and principal component analysis (PCA). As a result, there were 15 common peaks, 13 of which had been identified by LC-Q-TOF MS, and the similarity degrees of 15 batches of the samples was more than 0.9, and the samples were divided into 4 clusters by their quality difference. The method is reproducible, simple and reliablethat it can be used for quality control and evaluation of Resina Draconis from different manufacturers.
Chromatography, High Pressure Liquid
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methods
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Dracaena
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chemistry
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Drugs, Chinese Herbal
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analysis
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Principal Component Analysis
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Quality Control
3.Quality analysis of Guizhi Fuling capsule before and after application of in-process quality control in pharmaceutical production.
Jia-chun LI ; Jin-ling WANG ; Jing-ling WU ; Wen-zhe HUANG ; Zhen-zhong WANG ; Wei XIAO
China Journal of Chinese Materia Medica 2015;40(6):1017-1022
The effects of application of in-process quality control in Guizhi Fuling capsule production were evaluated by 192 batches data analysis. Using a statistical analysis method, each batch of data were to be counted to research for the difference between 96 samples adopting the technologies of in-process control or not. According to quality standards of Guizhi Fuling capsule, all measurements of the 192 batches of the drugs before and after the application of process control technology were analyzed, and they were within the rules. There was a significant difference between adopting the technologies of process control or not. Application of in-process control technology can improve the uniformity of lot-to-lot for Guizhi Fuling capsule.
Capsules
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chemistry
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Chemistry, Pharmaceutical
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Chromatography, High Pressure Liquid
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Drugs, Chinese Herbal
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chemistry
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Quality Control
4.Advance in research on chemical constituents from Notopterygii Rhizoma et Radix.
Shi-ping LI ; Long SHA ; Yi-wu ZHAO ; Zhi-liang XU ; Wen-zhe HUANG ; Zhen-zhong WANG ; Wei XIAO
China Journal of Chinese Materia Medica 2015;40(15):2952-2963
This paper summarized the recent 30 years research progress of the chemical constituents from Notopterygii Rhizoma et Radix. The chemical constituents from Notopterygii Rhizoma et Radix mainly consist of coumarins, polyene-polyacetylenes, sesquiterpenes, phenolic acids, while steroids and flavonoids were less reported. All constituents were confirmed and corrected through SciFinder. We also checked the Chinese name and English name and listed the CAS number of each compound. It can provide some guidelines for the research, development and utilization of Notopterygii Rhizoma et Radix in the future. Whether there is columbianin in the Notopterygii Rhizoma et Radix need to be further researched.
Apiaceae
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chemistry
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Drugs, Chinese Herbal
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analysis
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Rhizome
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chemistry
5.Chemical constituents from Artemisia annua.
Yi-wu ZHAO ; Fu-yong NI ; Ya-ling SONG ; Sheng-yang WANG ; Wen-zhe HUANG ; Zhen-zhong WANG ; Wei XIAO
China Journal of Chinese Materia Medica 2014;39(24):4816-4821
OBJECTIVETo investigate the chemical constituents of dried whole plants of Artemisia annua.
METHODThe chemical constituents were isolated by repeated silica gel chromatography, medium pressure column chromatography, and semi-preparative HPLC, and their structures were elucidated by spectroscopic analyses and comparison of NMR data with those reported in literature.
RESULT15 compounds were isolated and identified to be 5-O-[(E)-Caffeoyl] quinic acid(l), 1,3-di-O-caffeoylquinic acid(2), 4 5-di-O-caffeoylquinic acid(3), 3, 5-di-O-caffeoylquinic acid (4), 3, 4-di-O-caffeoylquinic acid (5), methyl-3,4-di-O-caffeoylquinic acid(6), methyl-3,5-di-O-caffeoylquinic acid(7), 3,6'-O-diferuloylsucrose(8), 5'-β-D-glucopyranosyloxyjasmonic acid(9), Scopoletin(10), scoparone (11), 4-O-β-D-glucopyranosyl-2-hydroxyl-6-methoxyacetophenone (12), chrysosplenol D (13), casticin (14), chrysosplenetin(15).
CONCLUSIONCompounds 2, 6, 8 and 9 are obtained from the Artemisia genus for the first time. Compounds 7 and 15 are obtained from this plant for the first time.
Artemisia annua ; chemistry ; Chromatography, Gel ; Chromatography, High Pressure Liquid ; Drugs, Chinese Herbal ; chemistry ; isolation & purification ; Flavonoids ; chemistry ; isolation & purification ; Medicine, Chinese Traditional ; Plants, Medicinal ; Quinic Acid ; analogs & derivatives ; chemistry ; isolation & purification ; Silica Gel
6.CT-guided percutaneous biopsy of musculoskeletal lesions
Xue-Bin ZHANG ; Xue-Zhe ZHANG ; Yan-Ning SHANG ; Zhen-Guo HUANG ; Wu WANG ; Wen HONG ; An REN ;
Chinese Journal of Radiology 2001;0(02):-
3 cm)and small lesions(diameter≤3 cm)were 80.6%(79/98)and 67.2% (45/67),respectively(P
7.Preparation of baicalein using thermophilic and sugar-tolerant beta-glucosidase.
Shi-ping LI ; Jian-hui WEN ; Yi-wu ZHAO ; Wen-zhe HUANG ; Jian-jun PEI ; Zhen-zhong WANG ; Lin-guo ZHAO ; Wei XIAO
China Journal of Chinese Materia Medica 2015;40(23):4616-4622
The reaction conditions of baicalin hydrolyzed into baicalein by a kind of thermophilic and sugar-tolerant beta-glucosidase were studied in this paper. The beta-glucosidase could catalyze baicalin into baicalein well in the acetic acid-sodium acetate buffer. The optimal enzyme activity was at 85 degrees C and pH 5.5. The enzyme was stable at the temperature less than 85 degrees C and pH range of 5-7.5. The maximum reaction rate V. and michaelis constant K. were 0.41 mmol x L(-1) x min(-1) and 3.31 mmol x L(-1) respectively. Different metal ions had different effects on the activity of enzyme. Na+ existing in acetic acid-sodium acetate buffer had an activation effect on enzyme. The enzyme activity was enhanced by the concentrations of glucose below 0.6 mol x L(-1), and was gradually inhibited when monosaccharide concentration was over 0.6 mol x L(-1). When the monosaccharide concentration reached 1.2 mol x L(-1), the inhibition rate of enzyme activity was about 50%, which showed good glucose tolerance. The good reaction conditions through the experiment have been determined as follows, the substrate: enzyme dose was 1 g: 0.2 mL, acetic acid-sodium acetate buffer pH 5.5, reaction temperature 85 degrees C, reaction time 10 h, and the enzymatic hydrolyzation ratio could reach 97%.
Biocatalysis
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Enzyme Stability
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Flavanones
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chemistry
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Flavonoids
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chemistry
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Glucose
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chemistry
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Hot Temperature
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Hydrolysis
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Kinetics
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beta-Glucosidase
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chemistry
8.New classification of Crowe type IV developmental dysplasia of the hip.
Hai-yang MA ; Yong-gang ZHOU ; Chong ZHENG ; Wen-zhe CAO ; Wang SEN ; Wen-ming WU ; Shang PIAO ; Yin-qiao DU
China Journal of Orthopaedics and Traumatology 2016;29(2):119-124
OBJECTIVETo compare differences between Crowe IV developmental dysplasia of the hip (DDH) with secondary acetabulum and Crowe IV DDH without secondary acetabulum,and determine whether it is necessary to divide Crowe IV DDH into two subtypes.
METHODSFrom June 2007 to May 2015,145 hips of 112 Crowe N patients who underwent total hip arthroplasty (THA) using S-ROM stem were divided into two groups: secondary acetabulum formaton group (group A) and no secondary acetabulum formaton group (group B). In group A,there were 12 females, 96 males,with an average age of (39.38 ± 11.19) years old. In group B, there were 2 females, 35 males, with an average age of (38.19 ± 10.92) years old. All the patients were evaluated by using Harris Hip Score. Radiographic evaluations were made preoperatively and during follow up. The differences between two groups were compared on dislocation height, canal flare index (CFI), subtrochanteric shortening osteotomy (SSTO) usage, pre- and post-operation Harris scores, complications.
RESULTSThe dislocation height for group A was (4.74 ± 1.57) cm, while the dislocation height for group B was (3.12 ± 1.15) cm. Significantly difference was detected between two groups. The CFI for group A was 2.69 ± 0.68, while the CFI for group B was 3.42 ± 0.79, and the significantly difference was detected between two groups. Harris scores were totally improved from 58.18 ± 15.67 preoperatively to 91.20 ± 3.79 post-operatively and the difference was significant. Pre-operative Harris scores was 58.1 ± 15.3 in group A, 58.3 ± 16.9 in group B. Post-operative Harris scores was 91.0 ± 4.1 in group A, 91.0 ± 5.1 in group B. No significant difference was found on Harris scores between A and B preoperatively and post-operatively. Complications of 4 cases peri-prosthesis fracture, 4 cases dislocation and 4 cases nerve injury occur in group A; While only one case dislocation and one case nerve injury occur in group B. No statistical significance was detected.
CONCLUSIONCrowe IV DDH with secondary acetabulum is significantly different from Crowe IV DDH without secondary acetabulum on dislocation height and femoral morphology, which causes the different selections of surgical techniques (SSTO usage or not). These important differences in fundamental parameters indicate the necessity to further divide Crowe IV DDH into IVA and IVB two subtypes.
Adolescent ; Adult ; Aged ; Female ; Hip Dislocation, Congenital ; classification ; surgery ; Humans ; Male ; Middle Aged ; Postoperative Complications ; therapy
9.Simultaneously preparation of grams of high purity tyrosol, crenulatin and salidroside from Rhodiola crenulata.
Xin LUO ; Xue-jing WANG ; Shi-ping LI ; Qiao ZHANG ; Yi-wu ZHAO ; Huang WEN-ZHE ; Zhen-zhong WANG ; Wei XIAO
China Journal of Chinese Materia Medica 2015;40(7):1300-1304
Tyrosol, crenulatin and salidroside are the main active constituents of Rhodiola crenulata, with extensive pharmacological activities. In the study, grams of high purity tyrosol, crenulatin and salidroside were simultaneously separated from R. crenulata by the first time. Firstly, R. crenulata was extracted by 70% alcohol. Then, with the yields of three compounds as the index, the macroporous resin was optimized. At last, grams of high purity tyrosol, crenulatin and salidroside were isolated by D-101 macroporousresin, purified by column chromatography. Detected by HPLC, the purity of three compounds were higher than 98%. This method has the advantages of simple process and operation, less dosage of organic solvent, highly yield and reproducibility, suitable for the simultaneously preparation of tyrosol, crenulatin and salidroside.
Chemical Fractionation
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methods
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Chemistry, Pharmaceutical
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Chromatography, High Pressure Liquid
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Coumarins
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analysis
;
isolation & purification
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Drugs, Chinese Herbal
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analysis
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isolation & purification
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Glucosides
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analysis
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isolation & purification
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Phenols
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analysis
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isolation & purification
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Phenylethyl Alcohol
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analogs & derivatives
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analysis
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isolation & purification
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Rhodiola
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chemistry
10.Application of molecularly imprinted technology for separation of PGG from Guizhi Fuling capsule.
Ya-ling SONG ; Xue-jing WANG ; Fu-yong NI ; Rui GU ; Yi-wu ZHAO ; Wen-zhe HUANG ; Zhen-zhong WANG ; Xiao-jie XU ; Wei XIAO
China Journal of Chinese Materia Medica 2015;40(6):1012-1016
1,2,3,4,6-penta-O-galloyl-D-glucose (PGG) is one of the main active compounds of Guizhi Fuling capsule. Molecularly imprinted polymers (MIP) have high affinity toward template molecules synthesized by molecularly imprinted technology for its specific combined sites, which can overcome the shortcoming of traditional separation methods, such as complex operation, low efficiency, using large quantity of solvent and environmental pollution. In this paper, surface molecularly imprinted polymer (SMIP) was prepared by surface imprinting with PGG as the template molecule. Its adsorption capacity was measured by the scatchard equation. The separation of PGG from Guizhi Fuling capsule at preparatived scale was achieved with molecularly imprinted polymer as stationary phase and the purity was 90.2% by HPLC. This method can be used to prepare PGG from Guizhi Fuling capsule with large capacity and is easy to operate. It provides a new method for efficient separation and purification for other natural products.
Adsorption
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Capsules
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chemistry
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Chromatography, High Pressure Liquid
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Drugs, Chinese Herbal
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chemistry
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Hydrolyzable Tannins
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chemistry
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isolation & purification
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Molecular Imprinting
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Polymers
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chemical synthesis
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chemistry