A sensitive and reliable liquid chromatography-electrospray ionisation-tandem mass spectrometry(LC-ESI-MS/MS)method was established to simultaneously quantitate four categories of compounds(isoflavonoids,flavonoids,al...A sensitive and reliable liquid chromatography-electrospray ionisation-tandem mass spectrometry(LC-ESI-MS/MS)method was established to simultaneously quantitate four categories of compounds(isoflavonoids,flavonoids,alkaloids and saponins)in Gegen-Qinlian decoction(GQD).These compounds were separated by a Shiseido CAPCELL PAK C18 column with a linear gradient consisting of 0.1%(v/v)formic acid in water(A)and 0.1%(v/v)formic acid in acetonitrile(B),and delivered at a flow rate of 0.3 mL/min.All the analytes were determined by electrospray positive ionization tandem mass spectrometry in a multiple reaction monitoring(MRM)mode.Linearity,accuracy,precision,recovery and stability of the method were evaluated with the validation over the range of 4.0-538 5 ng/mL.The proposed method was applied to the analysis of a Chinese herbal preparation GQD successfully.展开更多
采用微波辅助提取法,以50%乙醇作为提取剂,提取野菜鼠曲草中的黄酮类化合物,提取物经AB-8大孔树脂纯化后,利用高效液相色谱电喷雾离子化串联质谱(high performance liquid chromatography electrospray ionization tandem mass spectrom...采用微波辅助提取法,以50%乙醇作为提取剂,提取野菜鼠曲草中的黄酮类化合物,提取物经AB-8大孔树脂纯化后,利用高效液相色谱电喷雾离子化串联质谱(high performance liquid chromatography electrospray ionization tandem mass spectrometry,LC-ESI-MS/MS)结合标准品比对法对其组成进行分析,从中鉴定出8种黄酮和3种酚酸类化合物:3,5-二咖啡酰奎宁酸(4.957μg/mg)、绿原酸(2.144μg/mg)、奎宁酸(1.073μg/mg)、毛地黄黄酮(0.884μg/mg)、紫云英苷(0.777μg/mg)、金丝桃苷(0.486μg/mg)、芹菜素-7-葡萄糖苷(0.327μg/mg)、槲皮素-3-O-槐糖苷(0.144μg/mg)、槲皮素(0.072μg/mg)、木犀草苷(0.066μg/mg)和野黄芩苷(0.056μg/mg)。其中奎宁酸、芹菜素-7-葡萄糖苷、紫云英苷、槲皮素-3-O-槐糖苷在该植物中尚属首次发现。展开更多
A simple,sensitive and specilic liquid ehromatography-tandem mass spectrometry method was developed for simultaneous quantification of ezetimibe and simvastatin in rat plasma.The deuterium isotopes:ezetimibe d_4 and s...A simple,sensitive and specilic liquid ehromatography-tandem mass spectrometry method was developed for simultaneous quantification of ezetimibe and simvastatin in rat plasma.The deuterium isotopes:ezetimibe d_4 and simvastatin d_6 were used as internal standards for ezetimibe and simvastatin,respectively.MS/MS detection involved a switch of electron spray ionization mode from negative to positive at retention time 3.01 min.Samples were extracted from plasma by liquid-liquid extraction using tertiary butyl methyl ether.Chromatographic separation was achieved with Agilent Eclipse XBD-C_(18) column using mobile phase that consisted of a mixture of ammonium acetate(pH4.5:10 mM)-acetonilrile(25:75 v/v).The method was linear and validated over the concentration range of 0.2-40.0 ng/mL for simvastatin and 0.05-15.0 ng/mL for ezetimibe.The transitions selected were mlz 408.3→271.1 and mlz 4I2.0→ 275.10 for ezetimibe and ezetimibe d_4.and mlz 419.30→ 285.20 and mlz 425.40 →199.20 for simvastatin and simvastatin d_6.Intra- and inter-batch precisions for ezetimibe were 1.6-14.8%and 2.1-13.4%;and for simvastatin 0.94-9.56%and0.79-12%.respectively.The proposed method was sensitive,selective,precise and accurate for the quantification of ezetimibe and simvastatin simultaneously in rat plasma.The method was successfully applied to a pharmacokinetic study by oral co-administration of ezetimibe and simvastatin in SD rats.展开更多
Obesity can be considered as a chronic illness of epidemic proportion and its incidents have increased exponentially in recent years. The use of anti-obesity drugs such as sibutramine is somewhat helpful. There is a n...Obesity can be considered as a chronic illness of epidemic proportion and its incidents have increased exponentially in recent years. The use of anti-obesity drugs such as sibutramine is somewhat helpful. There is a need to quantify such drugs in biological samples, which is generally quite difficult. In this report, we developed and validated a simple, sensitive and specific liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the quantification of sibutramine (SB) and its two metabolites N-des methyl sibutramine (DSB) and N-di desmethyl sibutramine (DDSB) in human plasma. Zorbax SBC18 (4.6 mm 75 mm, 3.5 mm, 80 A) analytical column and 5 mM ammonium formate:acetonitrile (10:90, v/v) mobile phase were used for chromatographic separation of SB, DSB and DDSB. Multiple reaction monitoring (MRM) in the positive mode was used to detect SB, DSB and DDSB at m/z 280.3/124.9, 266.3/ 125.3 and 252.2/124.9, respectively. Liquid-liquid extraction was used for the extraction of analytes and internal standard from human plasma. This method was validated over a linear concentration range of 10.0-10,000.0 pg/mL for SB, DSB and DDSB with correlation coefficients (r) of Z0.9997. The drug and the two metabolites were stable in plasma samples. The validated method was successfully applied in a bioequivalence and pharmacokinetic study with human volunteers under fasting condition.展开更多
基金supported by the National Natural Science Foundation of China(No.90202039)"Chen Guang" Project for Personnel Cultivation of Shanghai Municipal Education Commission(No.09CG43)the Construction Program for Innovative Research Teamin Shanghai Institutions of Higher Education
文摘A sensitive and reliable liquid chromatography-electrospray ionisation-tandem mass spectrometry(LC-ESI-MS/MS)method was established to simultaneously quantitate four categories of compounds(isoflavonoids,flavonoids,alkaloids and saponins)in Gegen-Qinlian decoction(GQD).These compounds were separated by a Shiseido CAPCELL PAK C18 column with a linear gradient consisting of 0.1%(v/v)formic acid in water(A)and 0.1%(v/v)formic acid in acetonitrile(B),and delivered at a flow rate of 0.3 mL/min.All the analytes were determined by electrospray positive ionization tandem mass spectrometry in a multiple reaction monitoring(MRM)mode.Linearity,accuracy,precision,recovery and stability of the method were evaluated with the validation over the range of 4.0-538 5 ng/mL.The proposed method was applied to the analysis of a Chinese herbal preparation GQD successfully.
文摘采用微波辅助提取法,以50%乙醇作为提取剂,提取野菜鼠曲草中的黄酮类化合物,提取物经AB-8大孔树脂纯化后,利用高效液相色谱电喷雾离子化串联质谱(high performance liquid chromatography electrospray ionization tandem mass spectrometry,LC-ESI-MS/MS)结合标准品比对法对其组成进行分析,从中鉴定出8种黄酮和3种酚酸类化合物:3,5-二咖啡酰奎宁酸(4.957μg/mg)、绿原酸(2.144μg/mg)、奎宁酸(1.073μg/mg)、毛地黄黄酮(0.884μg/mg)、紫云英苷(0.777μg/mg)、金丝桃苷(0.486μg/mg)、芹菜素-7-葡萄糖苷(0.327μg/mg)、槲皮素-3-O-槐糖苷(0.144μg/mg)、槲皮素(0.072μg/mg)、木犀草苷(0.066μg/mg)和野黄芩苷(0.056μg/mg)。其中奎宁酸、芹菜素-7-葡萄糖苷、紫云英苷、槲皮素-3-O-槐糖苷在该植物中尚属首次发现。
文摘A simple,sensitive and specilic liquid ehromatography-tandem mass spectrometry method was developed for simultaneous quantification of ezetimibe and simvastatin in rat plasma.The deuterium isotopes:ezetimibe d_4 and simvastatin d_6 were used as internal standards for ezetimibe and simvastatin,respectively.MS/MS detection involved a switch of electron spray ionization mode from negative to positive at retention time 3.01 min.Samples were extracted from plasma by liquid-liquid extraction using tertiary butyl methyl ether.Chromatographic separation was achieved with Agilent Eclipse XBD-C_(18) column using mobile phase that consisted of a mixture of ammonium acetate(pH4.5:10 mM)-acetonilrile(25:75 v/v).The method was linear and validated over the concentration range of 0.2-40.0 ng/mL for simvastatin and 0.05-15.0 ng/mL for ezetimibe.The transitions selected were mlz 408.3→271.1 and mlz 4I2.0→ 275.10 for ezetimibe and ezetimibe d_4.and mlz 419.30→ 285.20 and mlz 425.40 →199.20 for simvastatin and simvastatin d_6.Intra- and inter-batch precisions for ezetimibe were 1.6-14.8%and 2.1-13.4%;and for simvastatin 0.94-9.56%and0.79-12%.respectively.The proposed method was sensitive,selective,precise and accurate for the quantification of ezetimibe and simvastatin simultaneously in rat plasma.The method was successfully applied to a pharmacokinetic study by oral co-administration of ezetimibe and simvastatin in SD rats.
文摘Obesity can be considered as a chronic illness of epidemic proportion and its incidents have increased exponentially in recent years. The use of anti-obesity drugs such as sibutramine is somewhat helpful. There is a need to quantify such drugs in biological samples, which is generally quite difficult. In this report, we developed and validated a simple, sensitive and specific liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the quantification of sibutramine (SB) and its two metabolites N-des methyl sibutramine (DSB) and N-di desmethyl sibutramine (DDSB) in human plasma. Zorbax SBC18 (4.6 mm 75 mm, 3.5 mm, 80 A) analytical column and 5 mM ammonium formate:acetonitrile (10:90, v/v) mobile phase were used for chromatographic separation of SB, DSB and DDSB. Multiple reaction monitoring (MRM) in the positive mode was used to detect SB, DSB and DDSB at m/z 280.3/124.9, 266.3/ 125.3 and 252.2/124.9, respectively. Liquid-liquid extraction was used for the extraction of analytes and internal standard from human plasma. This method was validated over a linear concentration range of 10.0-10,000.0 pg/mL for SB, DSB and DDSB with correlation coefficients (r) of Z0.9997. The drug and the two metabolites were stable in plasma samples. The validated method was successfully applied in a bioequivalence and pharmacokinetic study with human volunteers under fasting condition.
