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）,...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）.展开更多
The qualitative characterization and quantitative analysis of five bioactive flavonoids in Salix bordensis Turcz. were achieved via reversed-phase high-performance liquid chromatography coupled with diode array detect...The qualitative characterization and quantitative analysis of five bioactive flavonoids in Salix bordensis Turcz. were achieved via reversed-phase high-performance liquid chromatography coupled with diode array detection and tandem mass spectrometry, by using an Agilent ZORBAX SB-C18 HPLC column with a gradient elution of 0.3% (v/v) formic acid in water and methanol as the mobile phase. The compounds in the mixture were clearly identified by comparing their HPLC-DAD ultraviolet spectra, retention times, and MS data with those of corresponding reference compounds. All calibration curves showed good linearity (r2 > 0.9998) within the test ranges. The LOD, LOQ, specificity, precision, and accuracy for the method were validated. The results demonstrated that this analytical approach is ideal for the determination of bioactive compounds, such as flavonoids, and that it constructed a basis for the comprehensive evaluation of the quality of Salix bordensis Turcz.展开更多
Leaves of Ziziphus jujuba Mill.（Z. jujuba） were used as a folk medicine to treat children suffering from typhoid fever, furuncle and ecthyma in China. The present study was to establish a high performance liquid chr...Leaves of Ziziphus jujuba Mill.（Z. jujuba） were used as a folk medicine to treat children suffering from typhoid fever, furuncle and ecthyma in China. The present study was to establish a high performance liquid chroma- tography-diode array detector（HPLC-DAD） method for quality control of Z. jujuba leaves. The validated method was applied to the simultaneous characterization and quantification of sixteen main constituents in thirty samples, which comprised the whole life stage of Z. ]ujuba leaves from six cultivars in Yulin, Shannxi Province, China. HPLC fin- gerprint file of Z. jujuba leaves was set up and the results indicate that the major constituents of Z. jujuba leaves are （-）-catechin（1）, quercetin-3-O-robinobioside（3）, rutin（4） and quercetin-3-O-a-L-arabinosyl-（1---~2）-a-L-rhamnoside（6） with the total contents of the nine flavonoids in respective batch ranging from 18.52 mg/g to 39.51 mg/g. In addition, the contents of compounds depend on both the season and the cultivar. During ripening of Z. jujuba leaves, flavo- noids of all the cultivars present a similar trend： initially decrease from 25th, Jun. to 5th, Aug., 2015, and then in- crease for a period of time, finally slightly fluctuate on 5th Oct. The highest contents of total flavonoids were regis- tered on 25th Jun., 2015. Different cultivars have 50%--90% variation on the content for the three classes of com- pounds. Taken together, the results demonstrate that Z. jujuba leaves have great potential to be a new health-promoting resource based on flavonoids and the best sampling time of them is in June.展开更多
基金supported by program NCET Foundation,NSFC(30725045)the Special Program for New Drug Innovation of the Ministry of Science and Technology,China(2009ZX09311-001,2008ZX09101-Z-029)+1 种基金Shanghai Leading Academic Discipline Project(B906)by the Scientific Foundation of Shanghai,China(07DZ19728,09DZ1975700,09DZ1971500)
文摘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）.
文摘The qualitative characterization and quantitative analysis of five bioactive flavonoids in Salix bordensis Turcz. were achieved via reversed-phase high-performance liquid chromatography coupled with diode array detection and tandem mass spectrometry, by using an Agilent ZORBAX SB-C18 HPLC column with a gradient elution of 0.3% (v/v) formic acid in water and methanol as the mobile phase. The compounds in the mixture were clearly identified by comparing their HPLC-DAD ultraviolet spectra, retention times, and MS data with those of corresponding reference compounds. All calibration curves showed good linearity (r2 > 0.9998) within the test ranges. The LOD, LOQ, specificity, precision, and accuracy for the method were validated. The results demonstrated that this analytical approach is ideal for the determination of bioactive compounds, such as flavonoids, and that it constructed a basis for the comprehensive evaluation of the quality of Salix bordensis Turcz.
文摘Leaves of Ziziphus jujuba Mill.（Z. jujuba） were used as a folk medicine to treat children suffering from typhoid fever, furuncle and ecthyma in China. The present study was to establish a high performance liquid chroma- tography-diode array detector（HPLC-DAD） method for quality control of Z. jujuba leaves. The validated method was applied to the simultaneous characterization and quantification of sixteen main constituents in thirty samples, which comprised the whole life stage of Z. ]ujuba leaves from six cultivars in Yulin, Shannxi Province, China. HPLC fin- gerprint file of Z. jujuba leaves was set up and the results indicate that the major constituents of Z. jujuba leaves are （-）-catechin（1）, quercetin-3-O-robinobioside（3）, rutin（4） and quercetin-3-O-a-L-arabinosyl-（1---~2）-a-L-rhamnoside（6） with the total contents of the nine flavonoids in respective batch ranging from 18.52 mg/g to 39.51 mg/g. In addition, the contents of compounds depend on both the season and the cultivar. During ripening of Z. jujuba leaves, flavo- noids of all the cultivars present a similar trend： initially decrease from 25th, Jun. to 5th, Aug., 2015, and then in- crease for a period of time, finally slightly fluctuate on 5th Oct. The highest contents of total flavonoids were regis- tered on 25th Jun., 2015. Different cultivars have 50%--90% variation on the content for the three classes of com- pounds. Taken together, the results demonstrate that Z. jujuba leaves have great potential to be a new health-promoting resource based on flavonoids and the best sampling time of them is in June.
