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1.
Article in Chinese | WPRIM | ID: wpr-907157

ABSTRACT

Objective To establish a UHPLC method for the determination of zolpidem tartrate tablets after radiation, and to investigate the effect of different radiation doses on the content of zolpidem tartrate tablets. Methods Ultra high performance liquid chromatography was used. The content of zolpidem tartrate tablets irradiated by γ-ray was determined. Using C18 column, acetonitrile methanol-0.05 mol/L phosphoric acid solution (the pH value as 5.5 with triethylamine) (18∶26∶56) was used as the mobile phase. The flow rate was 0.7 ml/min, and the detection wavelength was 254 nm. Results The method validation showed good linearity in the concentration range of 5-80 μg/ml (r=0.999 6); The average recovery was 98.2%, RSD was 1.72%, and the repeatability was 0.87%. The contents of zolpidem tartrate were 105.1%, 106.4%, 102.7% and 105.4% under 0, 8, 25 and 80 kGy radiation. Conclusion UHPLC has accurate results with short analysis cycle in this study. It is suitable for the determination of zolpidem tartrate tablets after radiation. The content of zolpidem tartrate tablets remained basically unchanged after radiation.

2.
Article in Chinese | WPRIM | ID: wpr-907151

ABSTRACT

Objective To establish a method for the simultaneous determination of new mangiferin, mangiferin, artemisinin BⅡ, icariin and artemisinin A in Anemarrhenae Rhizoma by high performance liquid chromatography-evaporation light scattering detector (HPLC-ELSD). Methods The column was Agilent Poroshell 120 EC-C18. The mobile phase used acetonitrile-0.2% acetic acid water system with gradient elution. Column temperature was 30 ℃. Flow rate was 0.7 ml/min. Evaporative light scattering detector used nitrogen as atomizing gas. The atomizing gas temperature was 40 ℃ and the drift tube temperature was 90 ℃. The nitrogen volume flow rate was 2.00 L/min and the sample volume was 20 μl. Results The five components were able to achieve baseline separation. Neomangiferin, Mangiferin, Anemaponin BⅡ, Baohuoside I , Anemarrhena saponin AⅢwere determined as 24.1-386 μg/ml (r=0.999 3), 23.2-371 μg/ml (r=0.998 6), 54.2-867.2 μg/ml(r=0.995 6), 5.3-84.8 μg/ml (r=0.996 8), 10-160 μg/ml (r=0.998 9) respectively, which showed a good linear relationship within the concentration range. The average recovery rate of the five components was between 101.8% and 105.0%, and the repeatability RSD was less than 2.4%. The content of the above five components in Zhimu medicinal materials were 1.62%, 0.82%, 7.36%, 0.07%, 0.34%, respectively. Conclusion The method is simple, accurate, and highly sensitive, which could be used as the quantitative determination of multiple index components of Anemarrhenae Rhizoma.

3.
China Pharmacy ; (12): 26-31, 2022.
Article in Chinese | WPRIM | ID: wpr-907008

ABSTRACT

OBJECTIVE To improve the quality standard of T ibetan medicine of Qinjiaohua ,and to provide scientific basis for comprehensive quality evaluation. METHODS The qualitative analysis of 16 batches of Qinjiaohua with different producing areas and different origins was carried out by microscopic and TLC identification. According to the method stated in 2020 edition of Chinese Pharmacopoeia ,water content ,total ash content ,acid-insoluble ash content and alcohol-soluble extract content were determined. HPLC method was used to determine the contents of 5 components (loganic acid ,swertiamarin,gentiopicrin, swertionolin,isoorientin) in Qinjiaohua. RESULTS The medicinal powder of Qinjiaohua was light brown-yellow ,and the microscopic features of the powder were clear ,and pollen grains ,ducts,non-glandular hairs ,corolla epidermal cells and calyx epidermal cells were all found. The results of TLC indentification showed that there were fluorescent spots of the same color in the chromatogram of the tested product and the corresponding position of substance control (isoorientin). The content ranges of water content,total ash content ,acid-insoluble ash content and alcohol-soluble extract were 5.40%-8.87%,3.76%-6.40%,0.27%-0.58%, 26.81%-42.51%,respectively. The results of content determination methodology met the requirements of pharmacopoeia ;the content ranges of loganic acid ,swertiamarin,gentiopicrin,swertionolin and isoorientin in 16 batches of Qinjiaohua were 3.13-9.36,1.26-22.39,13.80-74.60,1.24-12.22,2.58-14.96 mg/g,respectively. CONCLUSIONS On the basis of the original quality standard of Qinjiaohua ,microscopic identification ,TLC identification ,content determination and examination items of water,total ash ,acid-insoluble ash and alcohol-soluble extract are added. It is preliminarily proposed that water content ,total ash content and acid-insoluble ash content should not exceed 9.0%,6.5% and 0.6%,while the contents of ethanol-soluble extract and gentiopicrin should not be less than 26.0% and 13.8 mg/g,respectively.

4.
China Pharmacy ; (12): 830-835, 2022.
Article in Chinese | WPRIM | ID: wpr-923189

ABSTRACT

OBJECTIVE To stu dy the effects of different processing me thods on the contents of the pharmacodynamic index components in Citrus aurantium and their antioxidant activity. METHODS According to the general principles of 2020 edition of Chinese Pharmacopoeia (volume Ⅳ) and the relevant processing methods in 2015 edition of Processing Specifications of Traditional Chinese Medicine in Zhejiang Province ,the samples of C. aurantium were prepared by steaming with water ,boiling with water ,stir-frying with vinegar ,stir-frying with wine ,stir-frying with bran ,processing with bran and processing with honey. The contents of moisture and ash in different products of C. aurantium were detected. The contents of naringin and neohesperidin in different products of C. aurantium were determined by high performance liquid chromatography. The antioxidant activity of different products was investigated by DPPH and ABTS + radical scavenging experiments and the total reducing power test. RESULTS The contents of moisture ,ash,naringin and neohesperidin were in line with the relevant requirements in 2015 edition of Processing Specifications of Traditional Chinese Medicine in Zhejiang Province . The content of naringin in descending order was as follow : unprocessed sample >sample processed with honey >sample processed with bran >sample boiled with water >sample stir-fried with vinegar>sample stir-fried with wine >sample stir-fried with bran >sample steamed with water. The content of neohesperidin in descending order was as follow :unprocessed sample >sample boiled with water >sample processed with bran >sample processed with honey >sample stir-fried with vinegar >sample steamed with water >sample stir-fried with wine >sample stir-fried with bran. The samples after boiling with water ,processing with bran ,and stir-fried with bran had better DPPH radicals scavenging ability (IC50 were 7.49,8.37 and 10.22 mg/mL,respectively). The samples after boiling with water ,steaming with water ,and processed with bran had better ABTS + radicals scavenging ability (IC50 were 1.76,2.03 and 2.72 mg/mL,respectively). In addition , compared with sample stir-fried with wine and processed with 发。E-mail:wanglu1286@163.com honey,unprocessed sample and other processed products of C.aurantium had bet ter total reducing ability. CONCLUSIONS After processing ,the contents of the main pharmacodynamic index components in C. aurantium have been reduced ,but they were also in line with the relevant requirements in 2015 edition of Processing Specifications of Traditional Chinese Medicine in Zhejiang Province . The antioxidant ability of some processed products has been enhanced.

5.
China Pharmacy ; (12): 808-812, 2022.
Article in Chinese | WPRIM | ID: wpr-923185

ABSTRACT

OBJECTIVE To establish the method for t he content determination of 5 active components in Yixin badiran jibuya granules and their fingerprints. METHODS High performance liquid chromatography method was adopted to determine the contents of luteolin- 7-O-β-D-glucuronide(LG),apigenin-7-O-glucuronide(APG),rosmarinic acid (RA),diosmetin-7-O-β-D-glucuronide (DG)and tilianin (TL)in 10 batches(No. S 1-S10)of Yixin badiran jibuya granules. The fingerprints of 10 batches of Yixin badiran jibuya granules were drawn by Similarity Evaluation System of Chromatographic Fingerprint of Traditional Chinese Medicine(2004 A edition ),and similarity evaluation and cluster analysis were also performed. RESULTS The contents of LG , APG,RA,DG and TL in 10 batches of Yixin badiran jibuya granules were 0.279 5-0.449 9,0.082 4-0.135 3,0.184 8-0.472 1, 0.149 0-0.332 6,0.311 2-0.623 3 mg/g,respectively. A total of 13 common peaks were demarcated in the fingerprints and were identified as LG (peak 2)APG(peak 6),RA(peak 7),DG(peak 8),TL(peak 11). The similarity ranged from 0.598 to 0.990. The results of cluster analysis showed that S 6-S10 were clustered into one category and S 1-S5 were clustered into one category. CONCLUSIONS Established method for content determination and fingerprints can be used for the quality control for Yixin badiran jibuya granules.

6.
Article in Chinese | WPRIM | ID: wpr-923031

ABSTRACT

Objective To establish a high performance liquid chromatography(HPLC) method for simultaneous determination of the contents of 7 components of chlorogenic acid, caffeic acid, paeoniflorin, ammonium glycyrrhizinate, baicalin, baicalein, and wogonin in Piqin oral liquid. Methods A double-wavelength HPLC method was performed. The column was Agilent Zorbax SB-C18 (250 mm × 4.6 mm, 5 μm). The mobile phase was 0.02% phosphoric acid aqueous solution (A)-acetonitrile (B) gradient elution; Flow rate: 1.0 ml/min; Column temperature: 35℃; Injection volume: 20 μl; Detection wavelength: 0-18.0 min, 325 nm (detect chlorogenic acid, caffeic acid); 18.0-65.0 min, 280 nm (detect paeoniflorin, baicalin, baicalein, ammonium glycyrrhizinate, wogonin). Results The chlorogenic acid, caffeic acid, paeoniflorin, ammonium glycyrrhizinate, baicalin, baicalein and wogonin were completely separated. Seven components have a good linear relationship between the peak area and concentration, with the recoveries between 96.41% and 99.70%. Conclusion This method is simple, accurate and reproducible, and can be used for the quality control of Piqin oral liquid.

7.
China Pharmacy ; (12): 718-723, 2022.
Article in Chinese | WPRIM | ID: wpr-923008

ABSTRACT

OBJECT IVE To provide reference for the improvement of the quality standard for Niushanggui capsules. METHODS Based on the previous quality standard ,thin-layer chromatography (TLC)identification methods were established for Angelicae dahurica and Anemarrhenae asphodeloides . High performance liquid chromatography (HPLC)method was established to determine the contents of 5 components simultaneously ,such as mangiferin ,prim-O-glucosylcimifugin,naringin,neohesperidin and 5-O-methylvisammioside. The limits were confirmed. RESULTS TLC chromatogram of Niushanggui capsules showed the same color spots in the same position as the corresponding (mixed)substance control or reference medicinal material of A. dahuricae and A. asphodeloides ,while the negative samples had no interference. The linear range of mangiferin ,prim-O-glucosylcimifugin, naringin,neohesperidin and 5-O-methylvisammioside were 7.98-127.63,6.74-107.84,53.06-848.96,39.31-628.90,13.54-216.62 μg/mL,respectively(all r=0.999 9). RSDs of precision ,stability(24 h)and repeatability tests were all no more than 1.20%(n= 6). The average recoveries were 95.00%,105.16%,97.16%,101.00% and 104.97%(RSD≤1.50%,n=6). In 4 batches of samples,the average contents of the above 5 components were 0.842,0.696,6.951,5.755 and 1.106 mg/g respectively ;the limits of A. asphodeloides ,Saposhnikovia divaricata and Citrus aurantium were based on the contents of mangiferin ,the total content of prim-O-glucosylcimmifugin and 5-O-methylvisammioside,naringin and neohesperidin ,which would not be less than 0.42,0.90 and 6.36 mg/grain,respectively. CONCLUSIONS TLC identification methods of A. dahurica and A. asphodeloides and the content determination methods of 5 components as mangiferin in Niushanggui capsules are established in this study ,and the limits of A. asphodeloides ,S. divaricata and C. aurantium are confirmed.

8.
China Pharmacy ; (12): 680-684, 2022.
Article in Chinese | WPRIM | ID: wpr-923002

ABSTRACT

OBJECTIVE To establis h the method for the simultaneous determination of six iridoids (loganic acid ,loganin, sweroside,dipsanoside B ,dipsanoside A ,sylvestroside Ⅰ)and one triterpene saponin (asperosaponin Ⅵ)in Dipsacus asper . METHODS High performance liquid chromatography (HPLC) method was adopted. The determination was performed on Symmetry® C18 column with mobile phase consisted of acetonitrile- 0.1% phosphoric acid solution (gradient elution )at the flow rate of 1.0 mL/min. The detection wavelengths were set at 212 nm(asperosaponin Ⅵ)and 237 nm(dipsanoside B ,dipsanoside A , sweroside,loganic acid ,sylvestroside Ⅰ,loganin). The column temperature was set at 30 ℃,and sample size was 20 μL. RESULTS The linear range of loganic acid , loganin, sweroside, sylvestroside Ⅰ , dipsanoside B , dipsanoside A and asperosaponin Ⅵ were 399.24-931.56,50.30-150.90,48.24-168.84,27.00-70.20,12.93-38.80,40.64-121.92,42.08-147.28 µg/mL (all r>0.999 0). RSDs of precision ,reproducibility and stability tests (24 h)were all less than 2%. Average recoveries were 104.43%(RSD=0.63%,n=6),101.74%(RSD=1.11%,n=6),100.76%(RSD=1.06%,n=6),98.00%(RSD=1.58%,n=6), 99.03%(RSD=2.31%,n=6),102.93%(RSD=2.26%,n=6),102.31%(RSD=1.00%,n=6),respectively,The contents were 142.5-280.6,5.5-49.0,28.0-112.9,7.2-35.8,4.4-16.9,17.2-79.3,0.8-54.5 mg/g,respectively. CONCLUSIONS Established method is accurate and reliable ,and can be used for the content determination of 7 components in D. asper .

9.
China Pharmacy ; (12): 586-591, 2022.
Article in Chinese | WPRIM | ID: wpr-920729

ABSTRACT

OBJECTIVE To establish HPLC finger print of Leonurus japonicus granules,and to determine the contents of 4 index components such as leonurine hydrochloride ,ferulic acid ,rutin,hyperoside. METHODS The determination was performed on Inertsil TM ODS-3 column with mobile phase consisted of acetonitrile (A)-0.1% formic acid solution (B)in the form of gradient elution;the flow rate was 1.0 mL/min,the detection wavelength was 280 nm,the column temperature was 25 ℃,and the sample size was 5 µL. Similarity Evaluation System of Chromatogram Fingerprint of TCM (2012 edition)was used for establishing the HPLC fingerprints of 10 batches of L. japonicus granules and analyzing their similarities. By comparing with HPLC fingerprints of reference substance ,the common peaks were identified. SPSS 25.0 and SIMCA 13.0 software were used for cluster analysis and principal component analysis ;the above HPLC method was used for the content determination of 4 index components in L. japonicus granules such as leonurine hydrochloride ,ferulic acid ,rutin,hyperoside. RESULTS HPLC fingerprints of 10 batches of L. japonicus granules were established ,and 16 common peaks were matched ,and 4 peaks identified were leonurine hydrochloride (peak 6),ferulic acid (peak 13),rutin(peak 14),hyperoside(peak 16);the similarities of 10 batches of samples were all higher than 0.970. The 10 batches of samples could be divided into four categories by cluster analysis and principal component analysis;the classification results were consistent. The contents of leonurine hydrochloride ,ferulic acid ,rutin and hyperoside were 122.10-138.82 μ g/g,9.33-10.45 μ g/g,14.12-18.95 μ g/g,5.87-8.06 μ g/g,respectively. CONCLUSIONS Established HPLC fingerprint of L. japonicus granules and the method for the content determination of 4 index components are simple and easy to operate,and have high precision and good repeatability ,which provide reference for the quality evaluation of L. japonicus granules.

10.
China Pharmacy ; (12): 555-562, 2022.
Article in Chinese | WPRIM | ID: wpr-920724

ABSTRACT

OBJECTIVE To optimize the existing t hin layer chromatography (TLC)identification and content determination methods of Jizhi syrup. METHODS High performance thin-layer chromatography (HPTLC)was used to identify five medicinal materials in Jizhi syrup ,such as Ilex chinensis ,Houttuynia cordata ,Peucedanum praeruptorum ,Citrus aurantium ,Glycyrrhiza uralensis. High performance liquid chromatography (HPLC)was used to determine the contents of procatechuic acid ,ephedrine hydrochloride and naringin in Jizhi syrup. RESULTS HPTLC results showed that the identification spots of pedunculoside , praeruptorin A ,naringin,and liquiritin were clearly displayed ,and the retention factors were in the range of 0.2 to 0.8. After validation,the method had been proved to be strongly specific ,robust and repeatable. HPLC results showed that the linear ranges of protocatechuic acid ,ephedrine hydrochloride and naringin were 4.32-431.67,1.14-114.17 and 7.02-702.33 μg/mL(all r> 0.996),respectively. The average recoveries were 100.61%,100.40% and 99.22%,and RSDs were all less than 2.00%. RSDs of precision(n=6),stability(24 h,n=7)and repeatability (n=6)were all less than 2.00%. The average contents of the three components in 10 batches were 623.3,152.1,1 213.9 μg/mL(RSD<10.00%),respectively. CONCLUSIONS In this study , HPTLC method of one-plate multi-drug is established for the identification of Jizhi syrup. One sample pretreatment method and two TLC conditions are used to realize the rapid identification of five kinds of medicinal materials. An HPLC method is established to determine the content of Jizhi syrup ,which realizes the fast quantification of three active components in Jizhi syrup ,and can be used to optimize the identification and content determination items in the existing legal quality standards of Jizhi syrup.

11.
China Pharmacy ; (12): 452-457, 2022.
Article in Chinese | WPRIM | ID: wpr-920462

ABSTRACT

OBJECTIVE To establish the fing erprint of Temurin- 5 powder,conduct chemical pattern recognition analysis ,and determine the contents of 4 components simultaneously. METHODS The fingerprints of 10 batches of Temurin- 5 powder were established and similarity evaluation was performed by using high performance liquid chromatography (HPLC)combined with the Similarity Evaluation System of Chromatographic Fingerprints of Traditional Chinese Medicine (2012 edition);common peaks were identified by comparing with mixed substance control. The common peaks were analyzed by systematic cluster analysis and principal component analysis with SPSS 26.0 software. The HPLC method was used to determine the contents of gallic acid , geniposide,chlorogenic acid and ellagic acid in 10 batches of samples. RESULTS A total of 15 common peaks were identified from the fingerprints of 10 batches of Temurin-5 powder,and the similarity was 0.997-0.999. It was identified that peak 1 was gallic acid ,peak 3 was geniposide ,peak 5 was chlorogenic acid and peak 12 was ellagic acid. Among the 10 batches of samples , S4 and S 9 were grouped into one category ,S6-S8 were grouped into one category ,and the other batches of samples were grouped into one category. The accumulative variance contribution rate of first three principal components was 89.245%. The linear ranges of gallic acid ,geniposide,chlorogenic acid and ellagic acid were 5.55-177.5,15.98-511.5,2.56-82.0 and 13.48-431.5 μg/mL, respectively. RSDs of precision ,stability(24 h)and repeatability tests were all less than 2%(n=6 or n=7). The average recoveries were 101.56%,102.21%,98.60% and 96.62%,respectively,RSDs were 1.90%,1.61%,1.58% and 1.73%(n=6). Average contents of above components were 5.03-5.64,10.38-12.16,1.40-1.69,6.47-7.11 mg/g,respectively. CONCLUSIONS The established fingerprint is stable and feasible ,and the content determination method meets the relevant regulations. Combined with chemical pattern recognition analysis ,it can be used for the quality control of Temurin- 5 powder.

12.
China Pharmacy ; (12): 280-286, 2022.
Article in Chinese | WPRIM | ID: wpr-913084

ABSTRACT

OBJECTIVE To establish H PLC fingerprint of Rheum palmatum before and after steaming with wine ,and to determine the contents of 3 differential components. METHODS HPLC method was used to establish the fingerprints of 15 batches of R. palmatum (before wine-steaming )and prepared rhubarb (after wine-steaming )and the similarity evaluation was conducted. The chemical pattern recognition analysis was carried out by principal component analysis ,cluster analysis ,partial least squares- discriminant analysis and orthogonal partial least squares-discriminant analysis. The contents of gallic acid ,resveratrol-4′-O- glucoside and resveratrol- 4′-O-(6″-galloyl)-glucoside in 30 batches of samples were determined. RESULTS In the fingerprint study,48 common peaks were demarcated for R. palmatum and 47 for prepared rhubarb as well as 17 common peaks were identified by reference substance. Cluster analysis and principal component analysis showed that R. palmatum derived from Qinghai before and after steaming with wine could be distinguished from those from Sichuan and Gansu. The results of content determination showed that the contents of 3 differential components in R. palmatum derived from Qinghai before and after steaming with wine were higher than those from other two production areas ;the contents of gallic acid in prepared rhubarb derived from those production areas were higher than R. palmatum ;the contents of resveratrol- 4′-O-glucoside and resveratrol- 4′-O- (6″-galloyl)-glucoside in R. palmatum derived from those production areas were higher than prepared rhubarb. CONCLUSIONS Fingerprint and content determination method established in this study can quickly ,scientifically and accurately evaluate the quality of R. palmatum from different producing areas before and after wine steaming ,which provide a basis for the processing specification and quality control of R. palmatum .

13.
Article in Chinese | WPRIM | ID: wpr-907672

ABSTRACT

Objective:To determinate the active ingredients and predicte action targets in Sanhua Decoction for treating cerebral ischemia based on HPLC and network pharmacology methods. Methods:The HPLC analysis was performed on HC-C18 (250 mm × 4.6 mm, 5 μm) with the mobile phase of methanolacetonitrile-0.05% phosphoric acid with gradient elution at the flow rate of 1.0 ml/min and 0.8 ml/min. The detection wavelength was set at 254 nm, the column temperature was at 30 ℃, and the injection volume was 10 μl. TCMIP v2.0 platform was used to search the action targets of rhein, emodin, chrysophanol, hesperidin, magnolol and notopterygiol. We used Cerebral ischemia as a keyword searching the databases such as Genecards, OMIM, TTD, and Disgenet to screen six potential targets for the treatment of cerebral ischemia by active ingredients, construct a protein interaction (PPI) network and a disease-component-target-pathway integration network.Results:The literature search determined that rhein, emodin, chrysophanol, hesperidin, magnolol and qianhuol were the index components for the determination of Sanhua Decoction. Their linear ranges were 0.080 4-0.804 0 μg, 0.015 3-0.382 0 μg, 0.041 8-0.626 4 μg, 0.312 6-3.908 0 μg, 0.037 9-0.568 8 μg, 0.045 3-1.359 6 μg, respectively. The correlation coefficient R 2 is greater than 0.999 0. The content ranges of the above six components in seven samples were 0.887-0.971 mg/g, 0.094-0.101 mg/g, 0.110-0.119 mg/g, 1.494-1.669 mg/g, 0.126-0.145 mg/g and 0.153-0.167 mg/g, respectively. Network pharmacology analysis found that the targets of the six components for the treatment of cerebral ischemia may be TNF, TP53, MAPK14, JUN, IL1B, MYC, ESR1, ICAM1, PTGS2, PPARG and so on. Conclusions:A quality control method forthe six active ingredients in Sanhua Decoction treating cerebral ischemia was established. This method is simple and repeatable. The ten potential targets of the six active ingredients in Sanhua Decoction for the treatment of cerebral ischemia have been clarified, laying a foundation for further research on the action mechanism.

14.
Acta Pharmaceutica Sinica ; (12): 3511-3517, 2021.
Article in Chinese | WPRIM | ID: wpr-906825

ABSTRACT

An ultra-high performance liquid chromatography method for the determination of 8 constituents in Qingzao Jiufei Decoction was established and the basis of related chemical substances with antioxidant activity in Qingzao Jiufei Decoction was explored. The separation was performed on a Waters Cortecs RP Shield C18 (150 mm × 2.1 mm, 1.6 μm) using UHPLC-DAD as the mobile phase was water (containing 0.1% phosphoric acid) – acetonitrile with flow rate of 0.30 mL·min-1 by gradient elution ① determining 5 constituents (amygdalin, liquiritin, liquiritin apioside, rutin and isoquercitrin) at the wavelength of 210 nm, 237 nm and 358 nm. Under gradient elution ②, 3 constituents (glycyrrhizin, glycyrrhizic acid and sesamin) were determined at the wavelength of 210 nm and 265 nm. The IC50 of 10 batches of Qingzao Jiufei Decoction scavenging 2,2'-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid) diammonium salt (ABTS+) free radicals obtained through test and Probit model was analyzed for correlation with the contents of 8 constituents. The established methods had a good linear relationship (r > 0.999), good repeatability and stability. The recovery rate was between 82.8% and 112.4%. In a series of concentration range, the higher the concentration of Qingzao Jiufei Decoction, the stronger the free radical scavenging effect. There was a significant correlation between the content of rutin and glycyrrhizic acid and the IC50 of scavenging free radicals. The content determination methods established in this experiment provide a basis for a reasonable and scientific evaluation of the quality of Qingzao Jiufei Decoction. Qingzao Jiufei Decoction has antioxidant activity, which is significantly positively correlated with the content of rutin and glycyrrhizic acid.

15.
China Pharmacy ; (12): 2994-3000, 2021.
Article in Chinese | WPRIM | ID: wpr-906780

ABSTRACT

OBJECTIVE:To compare the methods for the con tent determination of polysaccharide and reducing sugar in Polygonatum cyrtonema, and to optimize the wine-steaming technology of P. cyrtonema . METHODS : The contents of polysaccharide in P. cyrtonema were determined by anthrone-sulfuric acid method and phenol-sulfuric acid method. The contents of reducing sugar in P. cyrtonema were determined by anthrone-sulfuric acid method , phenol-sulfuric acid method and 3, 5-dinitrosalicylic acid (DNS)method,respectively. Taking appearance and property scores of processed products ,the contents of polysaccharide,reducing sugar and total sugar as indicators ,the amount of alcohol added ,steaming time and moistening time as factors,the wine-steaming technology of P. cyrtonema was optimized by Latin square design. The contents of polysaccharide , reducing sugar and total sugar were compared before and after steaming. RESULTS :The linear ranges of polysaccharide and reducing sugar obtained by anthrone-sulfuric acid method were both 0.006 6-0.033 mg/mL(R2=0.999 9). RSDs of precision , stability(90 min)and reproducibility tests were all lower than 3% and 2%,respectively. Average recoveries were 99.75%(RSD= 0.48%,n=6)and 103.40%(RSD=1.25%,n=6),respectively. The linear ranges of polysaccharide and reducing sugar obtained by phenol-sulfuric acid method were both 0.002 5-0.025 mg/mL(R2=0.999 2). RSDs of precision ,stability (90 min) and reproducibility tests were all lower than 5% and 6%,respectively. Average recoveries were 112.80%(RSD=2.36%,n=6)and 99.20%(RSD=3.47%,n=6). The linear range of reducing sugar obtained by DNS method was 0.01-0.18 mg/mL(R2=0.999 9). RSDs of precision ,stability(90 min)and reproducibility tests were all lower than 2%. Average recoveries was 96.95%(RSD= 1.19%,n=6). The optimal wine-steaming technology of P. cyrtonema included the amount of alcohol added of 20%,moistening time of 2 h and steaming time of 7 h. RSDs of average contents of polysaccharide ,reducing sugar and total sugar in wine-steamed products were all lower than 3% in 3 times of validation tests (n=3). The average contents of polysaccharide ,reducing sugar and total sugar in 4 batches of P. cyrtonema were 16.3%,11.2% and 27.4%;those of 4 batches of wine-steamed products were 3.4%, 61.0% and 64.4%,respectively. CONCLUSIONS :The anthrone- ) sulfuric acid method is the best for the determination of poly- saccharide in P. cyrtonema ;DNS method is the best for the pandongmei1228@126.com determination of reducing sugar in P. cyrtonema. The content ofpolysaccharide in wine-steamed products is decreased signifi- cantly,while the contents of reducing sugar and total sugar are increased significantly.

16.
China Pharmacy ; (12): 2970-2974, 2021.
Article in Chinese | WPRIM | ID: wpr-906776

ABSTRACT

OBJECTIVE:To establish a method for the simultaneous determination of eight constituents ,such as scopolin , scopoletin,chlorogenic acid ,cryptochlorogenic acid ,neochlorogenic acid ,isochlorogenic acid A ,isochlorogenic acid B ,and isochlorogenic acid C ,in different medicinal parts (stems,twigs and leaves )of Porana racemosa ,and to compare the contents of eight constituents . METHODS :HPLC method was adopted. The determination was performed on Agilent TC-C 18 column with mobile phase consisted of acetonitrile- 0.1% phosphate acid (gradient elution ) at the flow rate of 1.0 mL/min. The column temperature was 30 ℃,and the detection wavelength was set at 345 nm. The sample size was 10 μL. The contents of above constituents in stems ,twigs and leaves of P. racemosa were compared ,and the principal component analysis was carried out by Markerlynx XS software. RESULTS :The linear range of scopolin ,scopoletin,chlorogenic acid ,cryptochlorogenic acid , neochlorogenic acid ,isochlorogenic acid A ,isochlorogenic acid B ,and isochlorogenic acid C were 0.076 4- 7.64,0.062 8-6.28, 0.090 8-9.08,0.080 0-8.00,0.057 6-5.76,0.094 4-9.44,0.086 0-8.60,0.078 8-7.88 mg/L,respectively(all r>0.999). RSDs of precision,stability(24 h)and reproducibility tests were all lower than 2.0%. The average recoveries were 99.71%(RSD=1.36%, n=6),100.39%(RSD=1.76%,n=6),99.20%(RSD=1.75%,n=6),100.04%(RSD=2.63%,n=6),98.57%(RSD=1.99%, n=6),99.68%(RSD=1.84%,n=6),99.90%(RSD=1.88%,n=6),99.76%(RSD=1.47%,n=6),respectively. The average contents of above eight constituents were 9.725 3,1.286 5,7.271 3,1.347 6,0.997 7,0.710 9,0.656 3,0.364 7 mg/g in stems ; those were 0.690 3,0.411 7,4.394 3,0.639 6,0.531 3,1.392 7,0.989 1,1.129 2 mg/g in twigs ;those were 1.195 1,0.691 1, 27.952 9,6.173 4,1.405 1,0.549 7,0.288 8,0.794 2 mg/g in leaves ,respectively. The results of principal component analysis showed that different parts of P. racemosa could be divided into 3 categories. Among them ,most of the stems ofP. racemosa gathered in the first quadrant of score plot ,all the twigs gathered in the third quadrant , and all the leaves 分m gathered in the fourth quadrant. CONCLUSIONS :Established method is simple and reproducible ,and can be used for the determination of 8 constituents in different medicinal parts of P. racemosa. The average contents of neochlorogenic acid ,chlorogenic acid and cryptochlorogenic acid in the leaves of P. racemosa are relatively high ;the contents of isochlorogenic acid B ,isochlorogenic acid A and isochlorogenic acid C in the twigs are relatively high;the average contents of scopolin and scopoletin in the stems are also relatively high.

17.
Article in Chinese | WPRIM | ID: wpr-906217

ABSTRACT

Objective:Through comprehensive evaluation and analysis of the quality of Liuwei Dihuang (LWDH) preparations from different manufacturers and combining factors such as production technology, the key factors in the quality control of LWDH preparations are explored to provide a reference for improving the quality control level of LWDH preparations. Method:Morroniside, loganin and paeonol as quality control markers of LWDH products were determined by high performance liquid chromatography (HPLC), the mobile phase was acetonitrile (A) -0.3% phosphoric acid aqueous solution (B) for gradient elution (0-5 min, 5%-8%A; 5-20 min, 8%A; 20-35 min, 8%-20%A; 35-45 min, 20%-60%A; 45-55 min, 60%A), the detection wavelength of paeonol was at 274 nm, and the detection wavelengths of morroniside and loganin were at 240 nm. The quality characteristics of LWDH preparations with different dosage forms (big candied pills, water-honeyed pills, concentrated pills, hard capsules and soft capsules) from different manufacturers were analyzed. Combined these results with their actual production processes, the key-points of quality control in the whole production process were discussed. Result:The contents of three index ingredients in 128 batches of LWDH preparations were all in conformity with the standards of the 2015 edition of <italic>Chinese Pharmacopoeia</italic>, however, the content limit of some dosage forms in the current standard was unreasonable. For example, although the daily dose of crude drugs for big candied pills were almost twice the dose of water- honeyed pills (15.00, 8.57 g, respectively), they got exactly the same daily limits of the contents for both the quality markers. What′s more, these two formulations had the same process, so the differences between the process obviously could not be the reason of these differences. Conclusion:It is recommended that for the products with different dosage forms should have a similar content limits, if there are no obvious distinctions between their production processes. Which may benefit the quality control of the products with multi-dosage forms. The research on the quality standards of proprietary Chinese medicines should deeply study the existing characteristics of the quality standards, and fully respect the laws of the quality attributes of traditional Chinese medicines and the rules of the production process of Chinese patent medicines.

18.
China Pharmacy ; (12): 2743-2747, 2021.
Article in Chinese | WPRIM | ID: wpr-904777

ABSTRACT

OBJECTIVE:To establish the method for the content determination of 7 components,such as puerarin , 3′-methoxypuerarin,daidzein,rutin,hesperidin,salvianolic acid A and quercetin ,in Zhengxin jiangzhi tablets ,and conduct cluster heatmap analysis. METHODS :HPLC method was adopted. The separation was performed on Kromasil C 18 column with mobile phase consisted of acetonitrile- 0.1% formic acid solution (gradient elution )at the flow rate of 0.8 mL/min. The detection wavelength was set at 280 nm,and the column temperature was 25 ℃. The sample size was 10 μL. Taking the content data as the object,the cluster heatmap was drawn by Hiplot scientific research mapping platform. RESULTS :The linear range of puerarin , 3′-methoxypuerarin,daidzein,rutin,hesperidin,salvianolic acid A and quercetin were 17.00-170.00(r=0.999 9),5.14-51.40(r= 0.999 8),3.00-30.00(r=0.999 8),153.00-1 530.00(r=0.999 9),7.88-78.75(r=0.999 8),2.85-28.50(r=0.999 9)and 11.34-113.40 μg/mL(r=0.999 8),respectively. RSDs of precision ,stability(24 h)and repeatability tests were all less than 2%; the average recoveries were 99.58%(RSD=0.83%,n=6),100.31%(RSD=1.17%,n=6),100.61%(RSD=1.08%,n=6), 100.05%(RSD=0.82%,n=6),100.31%(RSD=1.38%,n=6),100.31%(RSD=0.85%,n=6),99.85%(RSD=1.01%, n=6),respectively. The contents of above components in 10 batches of samples were 7.262 5-8.941 5,2.464 9-3.068 9,1.478 9- 1.883 4,58.632 8-79.408 3,3.569 4-4.500 6,1.077 6-1.341 5,1.139 7-5.957 0 mg/g,respectively. Results of cluster heatmap analysis showed that 10 batches of samples could be divided into 4 categories,including S 1-S3 as one category ,S4 as one category,S5-S6 as one category and S 7-S10 as one category. CONCLUSIONS :The established method is simple ,accurate and specific,which can be used for the quality control of Zhengxin jiangzhi tablets ,combined with cluster heatmap analysis. There are some differences in the quality of different batches of samples.

19.
Article in Chinese | WPRIM | ID: wpr-921642

ABSTRACT

This study intends to develop a high performance liquid chromatography-diode array detection(HPLC-DAD) method for simultaneous determination of chlorogenic acid, 2-hydroxymethyl-3-hydroxyl-1-butene-4-O-β-D-(6″-O-caffeoyl)-glucopyranoside, pubescenoside B, huazhongilexone-7-O-β-D-glucopyranoside, rutin, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C in Ilex hainanensis. The HPLC conditions are as follows: Waters XBridge C_(18 )column(4.6 mm×250 mm, 5 μm), mobile phase of 0.5% formic acid in water(A)-acetonitrile(B), gradient elution(0-8 min, 5%-12% B; 8-18 min, 12%-18% B; 18-30 min, 18%-25% B; 30-40 min, 25%-30% B; 40-42 min, 30%-80% B; 42-45 min, 80% B) at the flow rate of 0.8 mL·min~(-1), detection wavelengths of 282, 324, and 360 nm, column temperature of 25 ℃, and injection volume of 5 μL. The content of the 8 phenols in 8 samples was 0.30-6.29, 0.29-3.27, 0.15-10.4, 0.51-5.85, 0.49-9.02, 0.51-4.68, 1.93-13.4, and 0.87-5.95 mg·g~(-1), respectively. Moreover, the content of phenols in the samples collected in October was higher than that of samples harvested in other months. The established method is accurate and sensitive for the determination of phenols in I. hainanensis, which is useful for the quality improvement of this herbal medicine.


Subject(s)
Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Ilex , Phenols
20.
China Pharmacy ; (12): 158-163, 2021.
Article in Chinese | WPRIM | ID: wpr-862637

ABSTRACT

OBJECTIVE:To establish fingerprint of Huafengdan yaomu ,and to determine the contents of 7 nucleosides in samples of different fermentation time. METHODS :HPLC method was adopted. The determination was performed on Pntulips BP-C18 column with mobile phase consisted of methanol-water (gradient elution )at the flow rate of 0.8 mL/min. The detection wavelength was set at 260 nm,and column temperature was 35 ℃. The sample size was 10 μL. Using xanthine as reference, HPLC fingerprint of 12 batches of Huafengdan yaomu was drawn. The similarity of samples were evaluated with Similarity Evaluation System of TCM Chromatographic Fingerprints (2012 edition). Common peaks were confirmed. The contents of uracil , hypoxanthine,xanthine,uridine,inosine,guanosine and thymidine were determined in samples of different fermentation time (0, 1,2,3,4 weeks)by the same method. RESULTS :There were 8 common peaks in 12 batches of Huafengdan yaomu ,with similarities ranging from 0.712 to 0.954;7 components were identified ,namely uracil ,hypoxanthine,xanthine,uridine,inosine, guanosine and thymidine. The linear ranges of mass concentrations of above 7 components in samples at different fermentation time were 0.87-8.7 μ g/mL (r=0.999 6), 4030 1.51-15.1 μg/mL(r=0.999 7),6.08-60.8 μg/mL(r=0.999 5), 号) 1.52-15.2 μg/mL(r=0.999 6),1.82-18.2 μg/mL(r=0.999 6), 1.48-14.8 μg/mL(r=0.999 6),1.63-16.3 μg/mL(r=0.999 3). The limits of quantification were 0.027 4,0.076 3,0.250 4,0.172 3,0.101 1,0.078 3,and 0.084 2 μ g/mL,and the detection limits were 0.008 7,0.025 5,0.007 9,0.084 1,0.035 7,0.026 9,0.027 5 μg/mL,respectively. RSDs of precision , repeatability and stability tests (12 h)were all less than 3%. The sample recovery rates were 94.16%-100.16%(RSD=2.24%,n= 6),93.87%-100.65%(RSD=2.67%,n=6),93.52%-99.66%(RSD=2.30%,n=6),93.67%-98.24%(RSD=1.89%,n=6), 96.00%-102.18%(RSD=1.96%,n=6),94.62%-101.54%(RSD=2.82%,n=6),97.72%-104.56%(RSD=2.97%,n=6). After fermentation for 0-4 weeks,the contents of the above 7 components and total nucleosides were 0.042-0.232,0.027-0.181, 0.039-0.651,0.026-0.225,0.034-0.111,0.009-0.124,0.079-0.099,0.647-1.292 mg/g,respectively. After fermentation for 1-4 weeks,the contents of uracil ,hypoxanthine,xanthine and total nucleosides were significantly increased ,compared with 0 week of fermentation;the contents of uridine ,inosine and guanosine were significantly lower than those in 0 weeks. CONCLUSIONS :The established fingerprint has strong characteristics and simple to operate ,which can be used for the quality control of Huafengdan yaomu;the content determination method is accurate and reliable ,and can be used to simultaneously determine the contents of 7 active nucleosides ;the content of nucleosides in Huafengdan muyao is affected by fermentation time.

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