ABSTRACT
A novel and sensitive HPLC-UV method has been developed for the simultaneous determination of twelve major compounds in Longdan Xiegan Pill.The chemical profile of the twelve compounds,including geniposidic acid (1),geniposide(2),gentiopicroside(3),liquiritin(4),crocin(5),baicalin(6),wogonoside(7),baicalein(8),glycyrrhizic acid (9),wogonin (10),oroxylin A ( 11 ) and aristolochic acid A (12),was acquired using high-performance liquid chromatography-diode array detector coupled with an electrospray tandem mass spectrometer (HPLC-DAD-ESI-MS).The analysis was performed on a Dikma Platisil ODS C18 column (250 mm × 4.6 mm,5 μm ) with a gradient solvent system of acetonitrile-0.1％ aqueous formic acid.The validation was carried out and the linearities ( r ＞ 0.9996),repeatability (RSD＜1.8％),intra- and inter-day precision (RSD＜1.3％),and recoveries (ranging from 96.6％ to 103.4％ ) were acceptable.The limits of detection (LOD) of these compounds ranged from 0.29 to 4.17 ng.Aristolochic acid A,which is the toxic ingredient,was not detected in all the batches of Longdan Xiegan Pill.Furthermore,hierarchical cluster analysis was used to evaluate the variation of the herbal prescription.The proposed method is simple,effective and suitable for the quality control of this traditional Chinese medicine (TCM).
ABSTRACT
A novel and sensitive HPLC-UV method has been developed for the simultaneous determination of twelve major compounds in Longdan Xiegan Pill.The chemical profile of the twelve compounds,including geniposidic acid（1）,geniposide（2）,gentiopicroside（3）,liquiritin（4）,crocin（5）,baicalin（6）,wogonoside（7）,baicalein（8）,glycyrrhizic acid（9）,wogonin（10）,oroxylin A（11）and aristolochic acid A（12）,was acquired using high-performance liquid chromatography-diode array detector coupled with an electrospray tandem mass spectrometer（HPLC-DAD-ESI-MS）.The analysis was performed on a Dikma Platisil ODS C18 column（250 mm×4.6 mm,5 μm）with a gradient solvent system of acetonitrile-0.1% aqueous formic acid.The validation was carried out and the linearities（r〉0.9996）,repeatability（RSD〈1.8%）,intra-and inter-day precision（RSD〈1.3%）,and recoveries（ranging from 96.6% to 103.4%）were acceptable.The limits of detection（LOD）of these compounds ranged from 0.29 to 4.17 ng.Aristolochic acid A,which is the toxic ingredient,was not detected in all the batches of Longdan Xiegan Pill.Furthermore,hierarchical cluster analysis was used to evaluate the variation of the herbal prescription.The proposed method is simple,effective and suitable for the quality control of this traditional Chinese medicine（TCM）.
ABSTRACT
Objective: To study materiomic release kinetics of Longdan Xiegan Pill. Methods: The materiomics release kinetics, the release profiles, and the multidimensional release characteristic of Longdan Xiegan Pill were determined by the paddle method with a rotate speed at 100 r/min in Chinese Pharmacopia, and the materiome was quantified by UV-vis combined Kalman filter method. Results: Longdan Xiegan Pill behaved typical sustained release profile which was consistent with Weibull and Higuchi release models. Conclusion: The sustained release profile of Longdan Xiegan Pill is depicted quantitatively by materiomic release dynamics in this paper, which demonstrates the obvious sustained release characteristic of the traditional pills.
ABSTRACT
AIM:To establish a HPLC method for determining simultaneously gentiopicroside and geniposide in Longdan Xiegan Pill(Radix et rhizoma Gentianae,Fructus Gardeniae,Radix Scutellariae,etc.).METHODS:C_ 18 column(5 ?m,4.6 mm?250 mm)was used.The mobile phase was methanol-water(23∶77).The detecting wavelength and the temperature of column were at 238 nm and at 40 ℃ respectively.RESULTS:The linear detection range of gentiopicroside was 3.03-30.30 ?g/mL(r=1.000 0),and the average recovery was 98.43%(RSD=1.08%).The linear detection range of geniposide was 9.76-97.60 ?g/mL(r=0.999 9),and the average recovery was 99.95%(RSD=0.91%).CONCLUSION:Two ingredients in Longdan Xiegan Pill could be determined simultaneously by this method which is convenient,rapid and accurate.It can be used for quality control in the production of Longdan Xiegan Pill.
ABSTRACT
AIM: To determine the dissolution of Longdan Xiegan Pills(Radix et Rhizoma Gentianae,Radix Scutellariae,Fructus Gardeniae,etc.) on the basis of markers such as gentiopicroside,baicalin and geniposide. METHODS: According to Appendix ⅩCⅢ of Chinese Pharmacopoeia 2005 edition VolⅡ,dissolution medium was 100 mL 0.5% SDS aqueous solution and rotating speed was 100 r/min.The dissolution solution of pill was taken and analyzed by HPLC method.A column of Kromasil C_(18)(4.6 mm?250 mm,5 ?m) was used.The mobile phase composed of A acetonitrile,B 1% glacial acetic acid aqueous solution,gradient eluation.The flow rate was 1.0 mL/min with the detection wavelength at 254 nm. RESULTS: The average dissolution of three batches of gentiopicroside,baicalin and geniposide exceeded the marker amount by factor of 0.75 time in 4 h. CONCLUSION: A reliable and qualitative method is established with good reproducibility for determination of dissolution of Longdan Xiegan Pills.