A reversed phase high performance liquid chromatography （HPLC） method was established for the simultaneous determination of 12, 13-dihydroxyeuparin and glycyrrhizic acid in Yanyanfang mixture. A Grace Apollo Cl8 col...A reversed phase high performance liquid chromatography （HPLC） method was established for the simultaneous determination of 12, 13-dihydroxyeuparin and glycyrrhizic acid in Yanyanfang mixture. A Grace Apollo Cl8 column （250 mm × 4.6 mm, 5 μm） was used as the stationary phase and the mobile phase was composed of acetonitrile and aqueous phosphoric acid （0.2%, v/v）. Gradient elution was carried out at the flow rate of 1.0 mL/min and the column temperature was 30 ℃. An ultraviolet （UV） detector was used with a selected wavelength of 240 nm. Calibration curves were linear within the concentration range of 4.6-45.75 μg/mL for 12, 13-dihydroxyeuparin （r〉0.9999） and 106.9-1068.9μg/mL for glycyrrhizic acid （r〉0.9999）, respectively. Recoveries were 102.18% for 12, 13-dihydroxyeuparin and 101.17% for glycyrrhizic acid. The method developed could be applied to the simultaneous determination of 12, 13- dihydroxyeuparin and glycyrrhizic acid in Yanyanfang mixture.展开更多
A simple and reliable high performance liquid chromatography （HPLC） method has been developed for the simultaneous quantification of five major bioactive components in ＇Shu-Jin- Zhi-Tong＇ capsules （SJZTC）, for t...A simple and reliable high performance liquid chromatography （HPLC） method has been developed for the simultaneous quantification of five major bioactive components in ＇Shu-Jin- Zhi-Tong＇ capsules （SJZTC）, for the purposes of quality control of this commonly prescribed traditional Chinese medicine. Under the optimum conditions, excellent separation was achieved, and the assay was fully validated in terms of linearity, precision, repeatability, stability and accuracy. The validated method was applied successfully to the determination of the five compounds in SJZTC samples from different production batches. The HPLC method can be used as a valid analytical method to evaluate the intrinsic quality of SJZTC.展开更多
A novel method for analysis of three active components curcumin, demethoxycurcumin and bisdemethoxycurcumin in Curcuma longa L. was developed by HPLC coupled with electrochemical detection. Three curcuminoids were wel...A novel method for analysis of three active components curcumin, demethoxycurcumin and bisdemethoxycurcumin in Curcuma longa L. was developed by HPLC coupled with electrochemical detection. Three curcuminoids were well separated on a C18 column and detected with high sensitivity. A mobile phase containing acetonitrile and 10 mM Na2HPO4-H3PO4 （pH 5.0） （50：50, v/v） was used. Good linearity was obtained in the range of 0.208-41.6, 0.197-39.4, and 0.227-114μM for curcumin, demethoxycurcumin and bisdemethoxycurcumin respectively. The limit of detection reached up to 10 ？ 8 M, which was lower than that by UV detection. The relative standard deviations （RSDs） ranged from 1.06%to 1.88%for intra-day precision and from 4.30%to 5.79%for inter-day precision, respectively. The proposed method has been applied in real herb sample and recoveries ranging from 86.3%to 111%were obtained.展开更多
In many areas of China Cirsium setosum is used as Cirsiumjaponicum DC. Although the two herbs have similar appearance and many similar compounds, they are totally different medicinal material, and have different pharm...In many areas of China Cirsium setosum is used as Cirsiumjaponicum DC. Although the two herbs have similar appearance and many similar compounds, they are totally different medicinal material, and have different pharmacodynamic actions. The fingerprint spectrum can be a good tool to distinguish the two herbs and control the quality of Cirsium japonicum DC. In this paper, the chemical fingerprint of Cirsiumjaponicum DC was established using raw materials from 15 origins in China. The chromatographic separations were obtained by a SHIM-PACK VP-ODS column （150 mm ~ 4.6 mm i.d., 5 ~tm） using gradient elution, and run time of 80 min. The peak of linarin was considered as the control peak. The experimental data were analyzed with the software of Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine （Version 2004A） and the quality control system of both the overall qualitative similari- ties and the overall quantitative similarities of traditional Chinese medicine chromatographic fingerprints.展开更多
建立了分析测定水环境中十氯酮的液相色谱-串联质谱法。水样经液液萃取、净化后，采用 Eclipse plus C18柱（100 mm×2.1 mm，3.5μm）分离，乙腈和水为流动相进行梯度洗脱，在电喷雾负离子多反应监测模式下进行检测，同位素内标法...建立了分析测定水环境中十氯酮的液相色谱-串联质谱法。水样经液液萃取、净化后，采用 Eclipse plus C18柱（100 mm×2.1 mm，3.5μm）分离，乙腈和水为流动相进行梯度洗脱，在电喷雾负离子多反应监测模式下进行检测，同位素内标法定量。结果表明：采用液相色谱-质谱联用技术，证实了十氯酮在甲醇中以半缩醛的形式存在，而在丙酮/乙腈中以偕二醇的形式存在。由于十氯酮极性较强，在净化时难以洗脱，并且不耐酸，所以不能与其他有机氯农药一起分析。十氯酮在5～100μg / L 范围有良好的线性关系，相关系数 r2=0.999，检出限及定量限分别为0.70 ng / L 和2.8 ng / L；在5、40和100 ng / L 3个浓度添加水平的平均回收率为95.1％～98.9％，相对标准偏差为3.85％～4.72％。本方法具有良好的灵敏度、回收率和重现性，适用于水环境中十氯酮的测定。展开更多
基金supported by Guangdong Natural Product Reference Material Research & Development Central Lab,the First Affiliate Hospital of Sun Yat-sen University and the Industry-University-Research Cooperation Program from Science and Technology Department of Guangdong Province (No:2010B090400533)
文摘A reversed phase high performance liquid chromatography （HPLC） method was established for the simultaneous determination of 12, 13-dihydroxyeuparin and glycyrrhizic acid in Yanyanfang mixture. A Grace Apollo Cl8 column （250 mm × 4.6 mm, 5 μm） was used as the stationary phase and the mobile phase was composed of acetonitrile and aqueous phosphoric acid （0.2%, v/v）. Gradient elution was carried out at the flow rate of 1.0 mL/min and the column temperature was 30 ℃. An ultraviolet （UV） detector was used with a selected wavelength of 240 nm. Calibration curves were linear within the concentration range of 4.6-45.75 μg/mL for 12, 13-dihydroxyeuparin （r〉0.9999） and 106.9-1068.9μg/mL for glycyrrhizic acid （r〉0.9999）, respectively. Recoveries were 102.18% for 12, 13-dihydroxyeuparin and 101.17% for glycyrrhizic acid. The method developed could be applied to the simultaneous determination of 12, 13- dihydroxyeuparin and glycyrrhizic acid in Yanyanfang mixture.
基金was funded by a grant from the Scientific and Technological Innovation Project Foundation of Shanxi China (No. 20090321099)
文摘A simple and reliable high performance liquid chromatography （HPLC） method has been developed for the simultaneous quantification of five major bioactive components in ＇Shu-Jin- Zhi-Tong＇ capsules （SJZTC）, for the purposes of quality control of this commonly prescribed traditional Chinese medicine. Under the optimum conditions, excellent separation was achieved, and the assay was fully validated in terms of linearity, precision, repeatability, stability and accuracy. The validated method was applied successfully to the determination of the five compounds in SJZTC samples from different production batches. The HPLC method can be used as a valid analytical method to evaluate the intrinsic quality of SJZTC.
基金supported by the National Scientific Foundation of China (Grant nos.21375101,90817103,and 30973672)Doctroral Fund of Ministry of Education of China (No.20110141110024)Innovation Seed Fund and Translational Medical Research Fund of Wuhan University School of Medicine
文摘A novel method for analysis of three active components curcumin, demethoxycurcumin and bisdemethoxycurcumin in Curcuma longa L. was developed by HPLC coupled with electrochemical detection. Three curcuminoids were well separated on a C18 column and detected with high sensitivity. A mobile phase containing acetonitrile and 10 mM Na2HPO4-H3PO4 （pH 5.0） （50：50, v/v） was used. Good linearity was obtained in the range of 0.208-41.6, 0.197-39.4, and 0.227-114μM for curcumin, demethoxycurcumin and bisdemethoxycurcumin respectively. The limit of detection reached up to 10 ？ 8 M, which was lower than that by UV detection. The relative standard deviations （RSDs） ranged from 1.06%to 1.88%for intra-day precision and from 4.30%to 5.79%for inter-day precision, respectively. The proposed method has been applied in real herb sample and recoveries ranging from 86.3%to 111%were obtained.
基金supported by the Main Program of Autonomous Region College Scientific Research Program (XJEDU2008145)
文摘In many areas of China Cirsium setosum is used as Cirsiumjaponicum DC. Although the two herbs have similar appearance and many similar compounds, they are totally different medicinal material, and have different pharmacodynamic actions. The fingerprint spectrum can be a good tool to distinguish the two herbs and control the quality of Cirsium japonicum DC. In this paper, the chemical fingerprint of Cirsiumjaponicum DC was established using raw materials from 15 origins in China. The chromatographic separations were obtained by a SHIM-PACK VP-ODS column （150 mm ~ 4.6 mm i.d., 5 ~tm） using gradient elution, and run time of 80 min. The peak of linarin was considered as the control peak. The experimental data were analyzed with the software of Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine （Version 2004A） and the quality control system of both the overall qualitative similari- ties and the overall quantitative similarities of traditional Chinese medicine chromatographic fingerprints.
文摘建立了分析测定水环境中十氯酮的液相色谱-串联质谱法。水样经液液萃取、净化后，采用 Eclipse plus C18柱（100 mm×2.1 mm，3.5μm）分离，乙腈和水为流动相进行梯度洗脱，在电喷雾负离子多反应监测模式下进行检测，同位素内标法定量。结果表明：采用液相色谱-质谱联用技术，证实了十氯酮在甲醇中以半缩醛的形式存在，而在丙酮/乙腈中以偕二醇的形式存在。由于十氯酮极性较强，在净化时难以洗脱，并且不耐酸，所以不能与其他有机氯农药一起分析。十氯酮在5～100μg / L 范围有良好的线性关系，相关系数 r2=0.999，检出限及定量限分别为0.70 ng / L 和2.8 ng / L；在5、40和100 ng / L 3个浓度添加水平的平均回收率为95.1％～98.9％，相对标准偏差为3.85％～4.72％。本方法具有良好的灵敏度、回收率和重现性，适用于水环境中十氯酮的测定。
