WANG Yin - hong, KANG A - long, FAN Bao - juan, SUN Wen - ji（1.Biomedicine Key Laboratory of Shaanxi Province, Northwest University, Xi＇an 710069, China 2. 451 Military Hospital of China, Xi＇an 710055, China; 3. Shaanxi Institute for Food and Drug Control, Xi＇an 710061, China）
Objective：To establish a quantitative method for the simultaneous determination of Huangjiangsu A, zingiberensis newsaponin and dioscin, and contrast the contents of three compounds in root of Dioscorea zingiberensis C. H. Wright from different habitats. Method：After refluxed with 70% ethanol, samples were separated by Diamonsil C18 column（250 mm×4.6 ram, 5 μm）;The mobile phase consisted of methanol（A） -water（B） with gradient elution（0- 10 rain, 78% A;10- 13 min, 78% A→90% A;13 -45 min, 90% A）,and the flow rate was 1.0 mL·min^-1. The temperature of drift tube and gas flow rate were 79.0℃ and 2.1 L·min^-1, respectively. Results：Huangjiangsu A, zingiberensis newsaponin and dioscin showed good linearity, and the average recoveries were 100. 4% , 103.0% and 95.3% , respectively. Conclusion： The method is simple and accurate for the simultaneous analysis of Huangjiangsu A, zingiberensis newsaponin and dioscin in root of Dioscorea zingiberensis.
关 键 词：盾叶薯蓣根 黄姜素A 盾叶新苷 薯蓣皂苷 HPLC-ELSD root of Dioscorea zingiberensis C. H. Wright Huangjiangsu A zingiberensis newsaponin diosein HPLC - ELSD 分 类 号： R917 [医药、卫生 > 药学 > 药物基础科学
JIA Yan-yan, LU Cheng-tao, SONG Ying, DING Li-kun, YANG Jing, CHEN Min-chun, LI Xue-qin,SONG Wei,ZHOU Lun,FENG Zhi-jun,WEN Ai-dong （Department of Pharmacy, the First Affiliated Hospital of Fourth Military Medical University of PLA , Xi＇ an 710032, China ）
Ivabradine and N-desmethylivabradine in human plasma was determined by high performance liquid chromatography coupled with tandem mass spectrometry （HPLC-MS/ MS）. Diazepam was used as internal standard. Ivabradine and N-desmethylivabradine was separated on a Diamosil C18 column （150 mm × 4. 6 mm × 5 μm）. Electrospray ionization （ESI） source was applied,and multiple reaction monitoring（MRM） mode was operated in the positive mode with the monitor ions at m/z 469.2→177.1 for ivabradine, m/z 455.2→177.1 for N-desmethylivabradine and m/z 285.1→193.1 for the internal standard, respectively. The linear calibration curve are obtained over the concentration range of 0. 101 3-quantitation are 0. 101 3 μg/L and 0. 085 μg/L for ivabradine and N-desmethylivabradine, respectively. The inter-day and intra-day precision （RSD） is less than 15%. The average recoveries are above 75%.
关 键 词：伊伐布雷定 去甲伊伐布雷定 高效液相色谱-串联质谱 血浆药物浓度 ivabradine N-desmethylivabradine high performance liquid chromatography coupled with tandem mass spectrometry （HPLC-MS/MS） plasma concentration
Objective：To establish an HPLC - MS method for the determination of telmisartan in human plasma. Method：The analyte was separated on a Diamonsil C18 （4.6 mm × 150 mm,5μm） analytical column. The mobile phase consisted of acetonitrile - water （contain 0.4% glacial acetic acid） （37 ： 63）and the/low rate was 0.95 ml/min, the/low rate of enter velocitron was 0.25 ml/ rain. Estazolam was used as internal standard. Result： The linear range of the plasma concentration of telmisartan was 3.0-1800μg·L^-1 and the limit of quantitative was 0.5 μg·L^-1. The relative recoveries of telmisartan were 91.95% - 102.87%. The RSD intra - day and inter - day were less than 5% and 10% respectively. Conclusion：This method is simple,selective and sensitive. It＇s suitable for the pharmacokinetic research of telmisartan in human plasma.
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