Aim The several species of the genus Paris called ＂Chonglou＂ are famous traditional Chinese herbal medicines. We established the quantitative analysis method of the steroidal saponins in some species of the genus Pa...Aim The several species of the genus Paris called ＂Chonglou＂ are famous traditional Chinese herbal medicines. We established the quantitative analysis method of the steroidal saponins in some species of the genus Paris and discussed their relations. Methods We detected the contents of 11 steroidal saponins in Paris samples with a Kromasel C18 （ 150 mm× 4.6 mm ID, 5μm） column which was subjected to gradient elution with acetonitrile-water （30：70- 60：40, V/V） at a flow rate of 1 mL· min^-1 by HPLC-ELSD and established chemical cluster tree using SPSS 11 software. Results All the samples could be separated and calibration curves of 11 saponins were prepared. We successfully detected the contents of 11 steroidal saponins in 14 Paris spp. in 30 min. The recovery for the assay of saponins was between 95 % and 97 %. The RSD of precision of 11 saponins and stability of samples were below 3 %. Chemical phylogenetic tree based on saponin contents indicated that 17 samples of Paris spp. clustered separately. Conclusion The established method is accurate and convenient, and suitable for the quantitative analysis of these 11 steroidal saponins in Paris spp.. The chemical phylogenetic tree is in accordance with Takhtajian classical taxonomy.展开更多
Aim Isolation and structural elucidation of the constituents from the aerialpart of Hypericum perforatum L. Methods Column chromatography and TLC were used to isolate chemicalconstituents. Physico-chemical characteriz...Aim Isolation and structural elucidation of the constituents from the aerialpart of Hypericum perforatum L. Methods Column chromatography and TLC were used to isolate chemicalconstituents. Physico-chemical characterization and spectroscopic analysis were employed forstructural identification. Results Three flavonols were isolated and identified. Conclusion Compound1 is a novel natural product and its structure has been characterized to be 3, 5, 7-trihydroxy-3',4'-isopropyldioxy-flavone.展开更多
In order to study the hydrolytic characterization of an anti-inflammatory prodrug （ RI-1 ） in vitro, an effective, accurate and reliable method for the simultaneous determination of the prodrug and its two hydrolyti...In order to study the hydrolytic characterization of an anti-inflammatory prodrug （ RI-1 ） in vitro, an effective, accurate and reliable method for the simultaneous determination of the prodrug and its two hydrolytic active compounds is developed using reverse phase high-performance liquid chromatography （RP-HPLC）. The chromatographic separation is performed on an ODS-2 C18 column （250 mm × 4. 6 mm, 5.0 μm particle size） with a simple elution program. The mobile phase is V（ methanol） ： V（0. 1% phosphoric acid solution） =90：10 （adjust pH to 2. 3）. A wavelength of 225 nm and a mobile phase flow rate of 1.0 mL/min are utilized for the quantitative analysis. Excellent linear behaviors over the investigated concentration ranges are observed with values of R2 higher than 0. 999 for all the analytes. The validated method is successfully applied to the simultaneous determination of the prodrug and its active components can be used to detect hydrolytic characterization in vitro.展开更多
An efficient method for quality control of Fructus Aurantii Immaturus (FAI),a famous traditional Chinese medicine (TCM) was established. A simple and reliable high-performance liquid chromatography-photodiode array de...An efficient method for quality control of Fructus Aurantii Immaturus (FAI),a famous traditional Chinese medicine (TCM) was established. A simple and reliable high-performance liquid chromatography-photodiode array detector (HPLC-DAD) procedure coupled with chemometric methods was developed for fingerprint analysis,qualitative analysis and quantitative determination of this herb. In qualitative and quantitative analyses,heuristic evolving latent projection (HELP) method was employed to resolve the overlapping peaks of the tested samples. Two bioactive components,namely hesperidin and naringin,are confirmed and determined,together with four flavonoids compounds tentatively identified including two new ones. From fingerprint analysis,the fingerprint data were processed with correlation coefficients for quantitative expression of their similarity and dissimilarity. The developed method based on an integration of chromatographic fingerprint and quantitative analysis is scientific,and the obtained results can be applied to the quality control of herb medicine.展开更多
For the purpose of obtaining small molecular and oxygen-containing aromatic compounds, taking a toluene-extracted coal pitch as the research object, the oxidation of coal-pitch by ozone （03） in formic acid was studi...For the purpose of obtaining small molecular and oxygen-containing aromatic compounds, taking a toluene-extracted coal pitch as the research object, the oxidation of coal-pitch by ozone （03） in formic acid was studied. The coal-pitch sample and the oxidized pitch residue were characterized by elementary analysis and Fourier transform infrared spectroscopy （FTIR）, while the small molecular products were analyzed by a gas chromatography-mass spectrometer （GC-MS）. The results show that the highest oxygen content of oxidized coal pitch had been acquired at a reaction temperature of 50℃C, an 03 flow rate of 6300 mg/h and a reaction time of 4 h. Quite a lot of hydroxyls and carbonyls were introduced into the structure of the oxidized coal-pitch, while the small molecules produced mainly involve nonpolar aro- matic compounds, aromatic anhydride and quinone compounds. It is speculated that the mechanism is direct electrophilic oxidation in which the molecules of 03 directly attack the aromatic ring at its carbon atoms with high electron density, and then generate hydroxyl or carbonyl until the aromatic ring cracks. This study shows that 03 can make the fused aromatic ring of coal-pitch become oxidized and depoly- merized, and hence the ozonization of coal-pitch can be a potential method for obtaining oxygen- containing aromatic compounds.展开更多
In order to reveal difference of phenolic substances and the content in the different varieties of pomegranate fruit and different mature period. The article uses 3 different fruit color phenotype （white, red, green...In order to reveal difference of phenolic substances and the content in the different varieties of pomegranate fruit and different mature period. The article uses 3 different fruit color phenotype （white, red, green） pomegranate cultivars as materials, the peel were determined by high performance liquid chromatography respectively （composition and content of phenolic compounds in the seeds and juice）. Results shows that the varieties of pomegranate peel and seeds were detected in 13 kinds of phenols, juice was detected in 12 type, and which did not detect epicatechin. At the same time, there was a significant difference in different parts of different varieties of pomegranate phenolic content.展开更多
Acetylspiramycin（ASPM）,a 16-membered basic macrolide antibiotic,is the acetylated derivative of spiramycin.In addition to the four main components,more than seventy minor components could be present in ASPM.Thus,it ...Acetylspiramycin（ASPM）,a 16-membered basic macrolide antibiotic,is the acetylated derivative of spiramycin.In addition to the four main components,more than seventy minor components could be present in ASPM.Thus,it is a challenge to obtain a baseline separation of ASPM components.Meanwhile,in some cases it was found that the results obtained by different brands of C_（18） columns were significantly different,indicating the necessity of a rational column selection for the separation of ASPM components.In this paper,we attempted to facilitate column selection for the analysis of ASPM using the database of the column characterization system established by Leuven University.With the CAPCELL PAK MG C_（18）（250 mm×4.6 mm,5μm） as the reference column,three groups of columns（F2 group：similar selectivity;2F6：intermediate ranked group;F6 group： different selectivity,compared to the reference column） were selected,and their performances in the separation of ASPM components were evaluated under the chromatographic conditions described in Chinese Pharmacopoeia monograph.A good relationship was demonstrated between the ranking of columns and their selectivity in the separation of ASPM components,indicating the column classification system established by Leuven University was a helpful tool in the selection of suitable columns for the analysis of ASPM,a complex mixture of basic compounds.展开更多
文摘Aim The several species of the genus Paris called ＂Chonglou＂ are famous traditional Chinese herbal medicines. We established the quantitative analysis method of the steroidal saponins in some species of the genus Paris and discussed their relations. Methods We detected the contents of 11 steroidal saponins in Paris samples with a Kromasel C18 （ 150 mm× 4.6 mm ID, 5μm） column which was subjected to gradient elution with acetonitrile-water （30：70- 60：40, V/V） at a flow rate of 1 mL· min^-1 by HPLC-ELSD and established chemical cluster tree using SPSS 11 software. Results All the samples could be separated and calibration curves of 11 saponins were prepared. We successfully detected the contents of 11 steroidal saponins in 14 Paris spp. in 30 min. The recovery for the assay of saponins was between 95 % and 97 %. The RSD of precision of 11 saponins and stability of samples were below 3 %. Chemical phylogenetic tree based on saponin contents indicated that 17 samples of Paris spp. clustered separately. Conclusion The established method is accurate and convenient, and suitable for the quantitative analysis of these 11 steroidal saponins in Paris spp.. The chemical phylogenetic tree is in accordance with Takhtajian classical taxonomy.
文摘Aim Isolation and structural elucidation of the constituents from the aerialpart of Hypericum perforatum L. Methods Column chromatography and TLC were used to isolate chemicalconstituents. Physico-chemical characterization and spectroscopic analysis were employed forstructural identification. Results Three flavonols were isolated and identified. Conclusion Compound1 is a novel natural product and its structure has been characterized to be 3, 5, 7-trihydroxy-3',4'-isopropyldioxy-flavone.
文摘In order to study the hydrolytic characterization of an anti-inflammatory prodrug （ RI-1 ） in vitro, an effective, accurate and reliable method for the simultaneous determination of the prodrug and its two hydrolytic active compounds is developed using reverse phase high-performance liquid chromatography （RP-HPLC）. The chromatographic separation is performed on an ODS-2 C18 column （250 mm × 4. 6 mm, 5.0 μm particle size） with a simple elution program. The mobile phase is V（ methanol） ： V（0. 1% phosphoric acid solution） =90：10 （adjust pH to 2. 3）. A wavelength of 225 nm and a mobile phase flow rate of 1.0 mL/min are utilized for the quantitative analysis. Excellent linear behaviors over the investigated concentration ranges are observed with values of R2 higher than 0. 999 for all the analytes. The validated method is successfully applied to the simultaneous determination of the prodrug and its active components can be used to detect hydrolytic characterization in vitro.
基金Project(20875104) supported by the National Natural Science Foundation of ChinaProject(10SDF22) supported by the Special Foundation of China Postdoctoral ScienceProject(201021200011) supported by the Advanced Research Plan of Central South University, China
文摘An efficient method for quality control of Fructus Aurantii Immaturus (FAI),a famous traditional Chinese medicine (TCM) was established. A simple and reliable high-performance liquid chromatography-photodiode array detector (HPLC-DAD) procedure coupled with chemometric methods was developed for fingerprint analysis,qualitative analysis and quantitative determination of this herb. In qualitative and quantitative analyses,heuristic evolving latent projection (HELP) method was employed to resolve the overlapping peaks of the tested samples. Two bioactive components,namely hesperidin and naringin,are confirmed and determined,together with four flavonoids compounds tentatively identified including two new ones. From fingerprint analysis,the fingerprint data were processed with correlation coefficients for quantitative expression of their similarity and dissimilarity. The developed method based on an integration of chromatographic fingerprint and quantitative analysis is scientific,and the obtained results can be applied to the quality control of herb medicine.
基金financially supported by the Key Project of Science and Technology of Universities of Henan Province (No.14A530003)the Key Project of Science and Technology of Henan Province (No.152102310090)
文摘For the purpose of obtaining small molecular and oxygen-containing aromatic compounds, taking a toluene-extracted coal pitch as the research object, the oxidation of coal-pitch by ozone （03） in formic acid was studied. The coal-pitch sample and the oxidized pitch residue were characterized by elementary analysis and Fourier transform infrared spectroscopy （FTIR）, while the small molecular products were analyzed by a gas chromatography-mass spectrometer （GC-MS）. The results show that the highest oxygen content of oxidized coal pitch had been acquired at a reaction temperature of 50℃C, an 03 flow rate of 6300 mg/h and a reaction time of 4 h. Quite a lot of hydroxyls and carbonyls were introduced into the structure of the oxidized coal-pitch, while the small molecules produced mainly involve nonpolar aro- matic compounds, aromatic anhydride and quinone compounds. It is speculated that the mechanism is direct electrophilic oxidation in which the molecules of 03 directly attack the aromatic ring at its carbon atoms with high electron density, and then generate hydroxyl or carbonyl until the aromatic ring cracks. This study shows that 03 can make the fused aromatic ring of coal-pitch become oxidized and depoly- merized, and hence the ozonization of coal-pitch can be a potential method for obtaining oxygen- containing aromatic compounds.
文摘In order to reveal difference of phenolic substances and the content in the different varieties of pomegranate fruit and different mature period. The article uses 3 different fruit color phenotype （white, red, green） pomegranate cultivars as materials, the peel were determined by high performance liquid chromatography respectively （composition and content of phenolic compounds in the seeds and juice）. Results shows that the varieties of pomegranate peel and seeds were detected in 13 kinds of phenols, juice was detected in 12 type, and which did not detect epicatechin. At the same time, there was a significant difference in different parts of different varieties of pomegranate phenolic content.
文摘Acetylspiramycin（ASPM）,a 16-membered basic macrolide antibiotic,is the acetylated derivative of spiramycin.In addition to the four main components,more than seventy minor components could be present in ASPM.Thus,it is a challenge to obtain a baseline separation of ASPM components.Meanwhile,in some cases it was found that the results obtained by different brands of C_（18） columns were significantly different,indicating the necessity of a rational column selection for the separation of ASPM components.In this paper,we attempted to facilitate column selection for the analysis of ASPM using the database of the column characterization system established by Leuven University.With the CAPCELL PAK MG C_（18）（250 mm×4.6 mm,5μm） as the reference column,three groups of columns（F2 group：similar selectivity;2F6：intermediate ranked group;F6 group： different selectivity,compared to the reference column） were selected,and their performances in the separation of ASPM components were evaluated under the chromatographic conditions described in Chinese Pharmacopoeia monograph.A good relationship was demonstrated between the ranking of columns and their selectivity in the separation of ASPM components,indicating the column classification system established by Leuven University was a helpful tool in the selection of suitable columns for the analysis of ASPM,a complex mixture of basic compounds.
