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1.
China Pharmacy ; (12): 961-966, 2021.
Article in Chinese | WPRIM | ID: wpr-876266

ABSTRACT

OBJECTIVE:To estab lish fingerprint of Duzhong butiansu pill s,analyze its chemical pattern recognition ,and determine the contents of 7 components in Duzhong butiansu pills ,so as to provide reference for the quality control of the preparation. METHODS :HPLC method was adopted. The determination was performed on Pntulips BP-C 18 Plus column with 0.2% phosphoric acid water-acetonitrile as mobile phase (gradient elution )at the flow rate of 1.0 mL/min. The detection wavelength was set at 330 nm,and column temperature was 35 ℃. The sample size was 20 μL. With paeonol as the reference,the HPLC fingerprints of 12 batches of Duzhong butiansu pills (S1-S12) were established with Similarity Evaluation System for TCM Chromatographic Fingerprint (2012 edition); common peaks were determined and the similarity was evaluated. The chromatographic peaks were identified by comparing with the reference substance. SPSS 21.0 and SIMCA 13.0 software were used for cluster analysis and principal component analysis ,and 22 common peaks were evaluated. The contents of the identified components in 12 batches of samples was determined by the above HPLC method. RESULTS :A total of 22 common peaks were identified in the HPLC fingerprint of 12 batches of Duzhong butiansu pills ,and the similarity was no loss than 0.960. There were 7 chemical components identified ,which were gallic acid (peak 1),chlorogenic acid (peak 3),liquiritoside(peak 6),hyperoside (peak 7),verbascoside(peak 8),icariin(peak 14)and paeonol (peak 15). Among the 12 batches of samples ,S1,S3-S5,S7, S9 and S 11 were classified as one category ,S2,S10 and S 124Y091 were clustered into one category ,S6 was one category and S was one category. The 22 common peaks were divided into three principal components. The characteristic value (15.130) and contribution rate (68.775%) of principal component 1 were the largest ,and the score coefficients of peak 3(0.305)and peak 4(0.298)were the highest. Among 12 batches of samples,the cont ents of above 7 components were 18.196 231.951 3,0.000 6-0.049 4,0.234 8-0.415 9,0.039 5-0.079 1,0.053 5-0.249 3,0.000 5-0.000 8,0.646 4-1.146 9 mg/g,respectively. CONCLUSIONS:HPLC fingerprint of Duzhong butiansu pills is established successfully. Twelve batches of samples are clustered into 4 category. Peak 3(chlorogenic acid )and peak 4(unknown)may be the important factors causing the difference of samples. The content of gallic acid is the highest among the 7 components.

2.
China Pharmacist ; (12): 384-388, 2018.
Article in Chinese | WPRIM | ID: wpr-705540

ABSTRACT

Objective:To explore the macroporous resin adsorption and the membrane separation technologies for the purification of saponins water extract of Anemarrhena asphodeloides. Methods:Ten-fold amount of water was used to extract twice for 120 min each time to extract saponins from Anemarrhena asphodeloides. The macroporous resin adsorption(HP-20,HPD-600,D101,AB-8) and the membrane separation technologies (ceramic microfiltration membranes 0.8 μm and 0.05 μm, and hollow fiber ultrafiltration mem-branes 50,10 and 6 kDa) were adopted to purify the saponins water extract liquid. The physicochemical parameters including electri-cal conductivity,viscosity and turbidity were measured,as well as the contents of total saponins,proteins and polysaccharides were de-termined. Results:The viscosity and turbidity decreased,the value of pH increased and the electrical conductivity of the saponins puri-fication liquid changed irregularly after the membrane filtration. The microfiltration membrane was more advantageous than the ultrafil-tration membrane in removing macromolecular substances. The smaller the pore diameter of microfiltration membrane, the smaller the intercepted molecular weigh,the higher the removal ratio of proteins and the higher the penetration rate of the total saponins,while the polysaccharides content was stable, which was consistent with the results of physicochemical parameters. The ceramic microfiltration membrane could obtain clearer extract,while the ultrafiltration membrane was more suitable for the enrichment of saponins when the in-tercepted molecular weight was 6 kDa. The macroporous resin HPD-600 was the best for the purification of timosaponin water extraction liquid.Conclusion:The selection of membrane for the separation and purification of different substances is particularly important. The change of physicochemical parameters and the content decrease of macromolecular substances have obvious corresponding relationship. Ultrafiltration membrane is better than microfiltration membrane for the purification of timosaponin water extract liquid.

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