RESUMEN
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）.
RESUMEN
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).
RESUMEN
A method for the determination of bisphenol A, octyphenol, nonylphenol in water samples was developed using stir bar sorptive extraction (SBSE) based on poly (vinylimidazole-divinylbenzene) monolithic material (SBSEM) combined with high performance liquid chromatography with diode array detection.To achieve the optimum extraction performance, several main extraction parameters, including extraction and desorption time, pH value and contents of inorganic salt in the sample matrix, were investigated.Under the optimized experimental conditions, the method showed good linearity and repeatability, low detection limits (S/N = 3) and quantification limits (S/N = 10) of the proposed method for the target compounds were achieved within the range of 0.13-0.66 and 0.44-2.19 μg/L, respectively.The extraction performance of SBSEM to the target compounds was also compared with commercial SBSE which used polydimethylsiloxane as coating.The proposed method was successfully applied to the determination of the target compounds in water samples.The recoveries of spiked target compounds in real samples ranged from 37.8%-101.1%.The results indicated that the developed method possessed advantages such as sensitivity, simplicity, low cost and high feasibility.
RESUMEN
Microwave-assisted extraction (MAE) was used for extraction of effective components of sarcandra glabra (Thunb.), and then chromatographic fingerprint of sarcandra glabra (Thunb.) was studied by high performance liquid chromatography/diode array detector (HPLC/DAD). The conditions of MAE were optimized by an orthogonal experiment, and then the authentication and validation of the chromatographic fingerprint were conducted. Nine peaks were identified as common peaks in the fingerprint chromatograms, and isofraxidin was considered as a reference compound and quantified. Relative standard deviations of retention time and peak area of each component were less than 3 % and 8 %, respectively. Similarity and difference analysis were conducted by use of PCA and relation coefficient. Twenty batches of sarcandra glabra (Thunb.) samples from two different producing areas could be classified into two different groups in the PCA model. The results showed that MAE-HPLC/DAD method was simple, efficient and stable for the study of complex chromatographic fingerprint of sarcandra glabra (Thunb.), which could provide more reliable and precise information for quality evaluation.
RESUMEN
Microwave-assisted extraction (MAE) was used for extraction of effective components of sarcandra glabra (Thunb.), and then chromatographic fingerprint of sarcandra glabra (Thunb.) was studied by high performance liquid chromatography/diode array detector (HPLC/DAD). The conditions of MAE were optimized by an orthogonal experiment, and then the authentication and validation of the chromatographic fingerprint were conducted. Nine peaks were identified as common peaks in the fingerprint chromatograms, and isofraxidin was considered as a reference compound and quantified. Relative standard deviations of retention time and peak area of each component were less than 3% and 8%, respectively. Similarity and difference analysis were conducted by use of PCA and relation coefficient. Twenty batches of sarcandra glabra (Thunb.) samples from two different producing areas could be classified into two different groups in the PCA model. The results showed that MAE-HPLC/DAD method was simple, efficient and stable for the study of complex chromatographic fingerprint of sarcandra glabra (Thunb.), which could provide more reliable and precise information for quality evaluation.