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RRLC-Q-TOF-MS法研究人参皂苷Rh1对映异构体在大鼠体内的药代动力学行为
引用本文:李春梅,于擎,孙乐,吴巍,郭迎迎,刘淑莹. RRLC-Q-TOF-MS法研究人参皂苷Rh1对映异构体在大鼠体内的药代动力学行为[J]. 质谱学报, 2014, 35(6): 509-515. DOI: 10.7538/zpxb.youxian.2014.0040
作者姓名:李春梅  于擎  孙乐  吴巍  郭迎迎  刘淑莹
作者单位:1.长春中医药大学,吉林省人参科学研究院,吉林 长春130117;2. 温州医科大学药学院,浙江 温州325035;3.中国科学院长春应用化学研究所,长春质谱中心,吉林 长春130022
基金项目:吉林省高校创新团队发展计划项目
摘    要:建立了高分离快速液相色谱-四极杆-飞行时间质谱(RRLC-Q-TOF-MS)法同时分离人参皂苷Rh1对映异构体,并研究其在大鼠体内的药代动力学行为。实验采用Agilent SB C18色谱柱,流动相A为水-乙腈(90∶10,V∶V)溶液,流动相B为水-乙腈(10∶90,V∶V)溶液,两种流动相内均含15 mmol/L甲酸铵,流速0.3 mL/min,进样量5 μL,二元线性梯度洗脱分离,在电喷雾负离子模式下进行质谱检测。结果表明,20-(S)和20-(R)人参皂苷Rh1的定量线性范围分别为0.24~39.00 mg/L和0.035~7.80 mg/L,定量限分别为0.20和0.03 mg/L,方法的检测限(S/N=3)分别为0.10和0.02 mg/L。精确度与精密度结果显示:两者的日内精确度分别为89.54%~95.79%和88.76%~94.33%,相对偏差小于5%;日间精确度分别为88.16%~92.41%和88.49%~94.35%,相对偏差小于5%。低、中、高3个浓度的提取回收率均大于90%。该方法可用于分离测定20-(S)和20-(R)人参皂苷Rh1,从而进行人参皂苷Rh1对映异构体在大鼠体内的药代动力学研究。

关 键 词:高分离快速液相色谱-四极杆-飞行时间质谱(RRLC-Q-TOF-MS)  人参皂苷Rh1  对映异构体  分离  药代动力学  

The Pharmacokinetics Studies of ginsenoside Rh1 Enantiomers in Rats by RRLC-Q-TOF-MS
LI Chun-mei,YU Qing,SUN Le,WU Wei,GUO Ying-ying,LIU Shu-ying. The Pharmacokinetics Studies of ginsenoside Rh1 Enantiomers in Rats by RRLC-Q-TOF-MS[J]. Journal of Chinese Mass Spectrometry Society, 2014, 35(6): 509-515. DOI: 10.7538/zpxb.youxian.2014.0040
Authors:LI Chun-mei  YU Qing  SUN Le  WU Wei  GUO Ying-ying  LIU Shu-ying
Affiliation:1. Jilin Ginseng Academy, Changchun University of Chinese Medicine, Changchun 130117, China; 2.Wenzhou Medical University, Wenzhou 325030, China; 3. Changchun Center of Mass Spectrometry, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022, China
Abstract:A method of rapid resolution liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry (RRLC-Q-TOF-MS) was developed for the simultaneous determination ginsenoside Rh1 enantiomers,and the pharmacokinetics of rats were studied. 20-(S) and 20-(R) ginsenoside Rh1 were separated on Agilent SB C18 column, using water acetonitrile(90∶10,V∶V)and water-acetonitrile(10∶90,V∶V),including 15 mmol/L ammonium formate as mobile phase A and B. The flow rate was 0.3 mL/min, and the injection volume was 5 μL. Determination was carried out by Q-TOF-MS in negative ion mode. The results show that the linearity of 20-(S) and 20-(R) ginsenoside Rh1 are 0.24-39.00 mg/L and 0.035-7.80 mg/L, respectively. The limits of quantification (LOQ) are 0.20 and 0.03 mg/L, the limits of detection (S/N=3) are 0.10 and 0.02 mg/L, respectively. The intra-day precisions are 89.54%-95.79% and 88.76%-94.33%, and relative deviations are less than 5%. The inter-day precisions are 88.16%-92.41% and 88.49%-94.35%, and the relative deviations are less than 5%. The recoveries of low, medium, and high concentrations are more than 90%. The method can be applied in separation and the pharmacokinetics studies of ginsenoside Rh1 enantiomers in rats.
Keywords:rapid resolution liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry (RRLC-Q-TOF-MS)  Rh1 enantiomers  separation  pharmacokinetics
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