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1.
Article in Chinese | WPRIM | ID: wpr-906366

ABSTRACT

Objective:To study the quality evaluation method of Cyperi Rhizoma processed with four excipients. Method:Ultra-performance liquid chromatography (UPLC) fingerprints of raw products and processed products with four excipients of Cyperi Rhizoma were established, and the changes of chemical components in the fingerprints before and after processing were compared by chemometric analysis. The mobile phase was consisted of methanol (A)-water (B) for gradient elution (0-10 min, 5%-40%A; 10-30 min, 40%-70%A; 30-40 min, 70%A) at a flow rate of 0.3 mL·min<sup>-1</sup>. The injection volume was 3 μL, the column temperature was 35 ℃, and the detection wavelength was 280 nm. The content changes of main index components in Cyperi Rhizoma before and after processing were compared by UPLC. The mobile phase was methanol-water (75∶25) and the detection wavelength was 242 nm. Result:Processing with four excipients had a significant impact on the overall characteristics of chemical components in the fingerprint of Cyperi Rhizoma. A total of 28 characteristic peaks were identified in fingerprints of the raw and processed products. Among them, peaks 1, 2 and 4 were specific peaks of the processed products, peak 5 was characteristic peak of the raw products. Peak 2 was identified as 5-hydroxymethylfurfural, peak 24 as cyperenone and peak 27 as <italic>α</italic>-cyperone. The 5-hydroxymethylfurfural produced by the processing with four excipients came from rice vinegar, rice wine and Maillard reaction of polysaccharides in Cyperi Rhizoma. The results of determination showed that there was no significant difference in the content of cyperenone after processing, but the content of <italic>α</italic>-cyperone decreased significantly. Conclusion:In the process of Cyperi Rhizoma processed with four excipients, there are new components produced by structural transformation, which are accompanied by changes in the content of index components. In this study, the quality of raw and processed products of Cyperi Rhizoma can be rapidly and effectively evaluated from qualitative and quantitative aspects.

2.
Chinese Pharmaceutical Journal ; (24): 2047-2053, 2018.
Article in Chinese | WPRIM | ID: wpr-858141

ABSTRACT

OBJECTIVE: To establish a quantitative analysis of multi-components by single-marker (QAMS) method for simultaneous determination of senkyunolide H, senkyunolide I, senkyunolide A, ligustilide, oxypaeoniflorin, albiflorin, paeoniflorin, benzoylpaeoniflorin and α-cyperone in Renshen Nüjin pills, in order to provide basis for studying its quality standards.METHODS: The analysis of the methanol extract of Renshen Nüjin pills was performed on Agilent Zorbax SB C18 column (4.6 mm×250 mm,5 μm), with mobile phase composed of methanol-acetonitrile (2∶1)-0.1% phosphoric acid solution at a flow rate of 0.9 mL•min-1 in gradient elution mode. The column temperature was maintained at 30 ℃, and the detection wavelengths were set at 280, 230 and 242 nm. Paeoniflorin was selected as the internal standard, and the relative correlation factors (RCF) of senkyunolide H, senkyunolide I, senkyunolide A, ligustilide, oxypaeoniflorin, albiflorin, paeoniflorin, benzoylpaeoniflorin and α-cyperone were determined by HPLC. The accuracy and feasibility of the method were validated by comparing the results of QAMS method and external standard method.RESULTS: The standard curves of senkyunolide H, senkyunolide I, senkyunolide A, ligustilide, oxypaeoniflorin, albiflorin, paeoniflorin, benzoylpaeoniflorin and α-cyperone had good linear relationship in the ranges of the tested concentrations. The precision, stability and repeatability complied with the requirements of methodology. The recoveries were 97.38%, 98.16%, 98.84%, 99.63%, 97.04%, 99.14%, 100.04%, 96.93% and 98.48%, RSDs were 1.38%, 1.18%, 0.97%, 0.86%, 1.68%, 1.30%, 0.57%, 1.32% and 1.19%, respectively. No significant differences were observed in the determination results by QAMS method and external standard method.CONCLUSION: The QAMS method can be used for the content determination and quality control of the nine components in Renshen Nüjin pills.

3.
Article in Chinese | WPRIM | ID: wpr-852616

ABSTRACT

Objective: To establish HPLC coupled with wavelength switching and gradient elution method (HPLC-DVD) for simultaneous determination of nine main components (α-cyperone, genipin-1-β-D-gentiobioside, geniposide, crocin I, senkyunolide H, senkyunolide I, senkyunolide A, ligustilide, and atractylodin) in Yueju Tablets. Methods: The chromatographic separation was achieved on Zorbax Eclipse Plus C18 (250 mm × 4.6 mm, 5 μm) column with methanol-acetonitrile (2∶1) (A)-0.2% glacial acetic acid solution (B) as mobile phases for gradient elution, at the flow rate of 0.9 mL/min; The detection wavelength was set at 240 nm for α-cyperone, genipin-1-β-D-gentiobioside and geniposide, 440 nm for crocin I, 280 nm for senkyunolide H, senkyunolide I, senkyunolide A and ligustilide, and 340 nm for atractylodin. The volume of sample injection was 10 μL. Results: The nine active components were well separated and showed good linearity, such as α-cyperone 2.58—51.60 μg/mL (r = 0.999 4), genipin-1-β-D- gentiobioside 11.99—239.80 μg/mL (r = 0.999 9), geniposide 17.96—359.20 μg/mL (r = 0.999 6), crocin-I 3.98—79.60 μg/mL (r = 0.999 7), senkyunolide H 2.82—56.40 μg/mL (r = 0.999 9), senkyunolide I 2.38—47.60 μg/mL (r = 0.999 9), senkyunolide A 6.04—120.80 μg/mL(r = 0.999 5), ligustilide 7.98—159.60 μg/mL (r = 0.999 3), and atractylodin 6.51—130.20 μg/mL (r = 0.999 2). The precision was good, and RSD was not more than 1.22%. The repeatability was good, and RSD was not more than 1.75%. The stability was good in 18 h, and RSD was not more than 1.37%. The average recoveries and corresponding RSD values were 97.64% (0.98%), 99.09% (1.46%), 100.11% (1.03%), 97.87% (0.80%), 98.59% (1.19%), 96.89% (1.34%), 99.38% (0.58%), 98.50% (1.22%), and 99.71% (0.85%), respectively. The contents of 10 batches of α-cyperone, genipin-1-β-D-gentiobioside, geniposide, crocin I, senkyunolide, H, senkyunolide I, senkyunolide A, ligustilide and atractylodin were 0.282—0.344, 2.099—2.445, 3.628—4.225, 0.758—0.913, 0.241—0.286, 0.217—0.266, 1.077—1.291, 1.386—1.623, and 1.137—1.434 mg/tablet. Conclusion: HPLC coupled with wavelength switching and gradient elution method has been established for simultaneous determination of nine components in Yueju Tablets. The method is simple, quick, accurate, and it can be used for content determination and quality control of Yueju Tablets.

4.
Article in Chinese | WPRIM | ID: wpr-580308

ABSTRACT

AIM: To establish the analytical methods for determing paeoniflorin,paeonol and ?-cyperone in Baixiangdan Capsule(extract of Radix Paeoniae alba,extract of paeonol,volatile oil of Rhizoma Cyperi). METHODS: The contents of paeoniflorin,paeonol and ?-cyperone in the capsule were determined by HPLC respectively. RESULTS: The linear range of paeoniflorin was within 0.6125.508 ?g(r=(0.999 3)) and the average recovery was 98.16%(RSD=1.18%,n=5).The linear range of paeonol was 0.150 4 ?g-1.353 6 ?g(r=(0.999 8)) and the average recovery was 98.16%(RSD=1.52%,n=5).The linear range of ?-cyperone was(0.271)-2.439 ?g(r=(0.999 9)) and the average recovery was 98.02%(RSD=1.58%,n=5). CONCLUSION: The method is reliable,accurate,feasible and reproducible and can be applied to the quality control of Baixiangdan Capsule.

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