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1.
China Journal of Chinese Materia Medica ; (24): 3070-3077, 2019.
Article Dans Chinois | WPRIM | ID: wpr-773188

Résumé

In order to evaluate the quality of Styrax more comprehensively,this study attempted to establish an HPLC wavelength switching method to simultaneously determine the content of seven compounds in Styrax,and chemometrics were used to analyze the quality difference between different sources of Styrax,and finally establish a characteristic chromatogram of Styrax. The column was Agilent ZORBAX Extend C18( 4. 6 mm×250 mm,5 μm) with phase a mixture of acetonitrile-0. 1% phosphoric acid aqueous solution as the mobile phase in a gradient elution procedure; the detection wavelength was set as follows: 0-13. 5 min,194 nm( benzoic acid);13. 5-20. 5 min,278 nm( cinnamic acid); 20. 5-32 min,194 nm( benzyl benzoate,benzyl cinnamate,cinnamyl cinnamate,dehydroabietic acid); 32-55 min,241 nm( abietic acid). The methodological verification results showed that when the injection masses of benzoic acid,cinnamic acid,benzyl benzoate,benzyl cinnamate,cinnamyl cinnamate,dehydroabietic acid and abietic acid were0. 006 948-0. 694 8,0. 001 426-0. 142 6,0. 013 16-0. 658 0,0. 006 148-0. 614 8,0. 008 035-0. 803 5,0. 002 121-0. 212 1,and0. 010 172-1. 017 2 μg,respectively,there were good linear relationship between injection mass and peak area. The average recovery rates of seven compounds were in the range from 94. 34% to 105. 8%,and all RSD were less than 3. 0%( n = 6). The methodological verification results showed that the developed HPLC wavelength switching method has good accuracy and repeatability. The results of the sample analysis showed that the quality of Styrax from different sources was quite different. The chromatogram of Styrax reference material( S1) was used as the reference chromatogram to calculate the fingerprint similarity of each batch of samples. The results showed that the similarities of samples S2-S10 were 0. 952,0. 949,0. 981,0. 351,0. 751,0. 969,0. 979,0. 992 and 0. 971,respectively.The similarity values of other batches samples were satisfactory,except for sample S5 and S6,indicating that the quality difference among these samples is small. The similarity values of S11-S20 were 0. 060,0. 055,0. 054,0. 285,0. 092,0. 002,0. 044,0. 044,0. 044,and 0. 040,respectively. The results showed that compared with the sample S1,there was a large quality difference among S11-S20. Based on the chromatograms of S1-S10,the HPLC characteristic chromatograms of Styrax was established and the purpose is to give reference to other pharmaceutical researchers. The newly developed HPLC wavelength switching method have the advantages of simplicity,reproducibility and specificity,and the developed HPLC characteristic chromatograms provided a reference method for the overall quality evaluation of Styrax.


Sujets)
Chromatographie en phase liquide à haute performance , Médicaments issus de plantes chinoises , Composés phytochimiques , Contrôle de qualité , Reproductibilité des résultats , Styrax , Chimie
2.
Chinese Traditional Patent Medicine ; (12): 601-604, 2018.
Article Dans Chinois | WPRIM | ID: wpr-710221

Résumé

AIM To establish an HPLC method for the simultaneous content determination of berberine hydrochloride,baicalin,baicalein,wogonin,aloe emodin,rhein,emodin,chrysophanol,physcion in Sanhuang Tablets (Rhei Radix et Rhizoma,Scutellariae Radix,berberine hydrochloride).METHODS The analysis of methanol extract of this drug was performed on a 35 ℃ thermostatic Waters sunfire C1s column (4.6 mm ×250 mm,5 μm),with the mobile phase comprising of methanol-acetonitrile-0.1% phosphoric acid flowing at 1.0 mL/min in a gradient elution manner,and the detection wavelength was set at 254 nm.RESULTS Nine constituents showed good linear relationships within their own ranges (r > 0.999 0),whose average recoveries were 99.03%-100.03% with the RSDs of 0.63%-1.07%.The contents of various constituents in ten batches of samples demonstrated obvious differences.CONCLUSION We should pay attention to the unstable quality of Sanhuang Tablets.

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