HPLC-MS法同时测定红竹海狗丸中4种成分的含量  

HPLC-MS simultaneous determination of four constituents in Hongzhu Callrhinus pills

作　　者：张振[1] 魏春敏[2] 袁桂艳[2] 王本杰[2] 张蕊[2] 郭瑞臣[2] 

机构地区：[1]山东大学药学院,济南250012 [2]山东大学齐鲁医院临床药理研究所,济南250012

出　　处：《药物分析杂志》2009年第11期1812-1816,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立高效液相色谱-质谱法同时测定中药复方制剂红竹海狗丸中人参皂苷Rg1、淫羊藿苷、补骨脂素和异补骨脂素的含量。方法:固定相为Agilent Tc-C18(4.6 mm×250 mm,5μm),流动相为0.1%醋酸和乙腈,梯度洗脱,流速为1.0 mL.min-1;ESI+,选择性监测(SIM)质荷比(m/z)为209,321,677,823的离子对,内标为劳拉西泮。结果:人参皂苷Rg1、淫羊藿苷、补骨脂素和异补骨脂素分别在2.02～12.12,2.0～12.0,0.53～1.86,0.4～1.4μg.mL-1浓度范围内线性关系良好。红竹海狗丸每丸分别含人参皂苷Rg1(232.6±0.64)μg、淫羊藿苷(669.0±14.51)μg、补骨脂素(564±34.71)μg和异补骨脂素(428±20.17)μg。结论:所建立的方法方便、快捷、稳定,可同时测定红竹海狗丸多种成分含量。结果准确可靠,可用于红竹海狗丸的制剂质量控制,为其人体药动学研究提供依据。Objective：To establish a high-performance liquid chromatography-mass spectrum method for determination of panaxsaponin Rg1, icariin, psoralen and isopsoralen in Hongzhu Callrhinus pills. Methods：An Agilent Tc-C18 （4.6 mm×250 mm,5 μm） column was used for the separation, and gradiently eluted by 0.1% acetic acid-acetonitrile with flow rate of 1.0 mL·min^-1. AP-ESI with positive ion mode and the selected ion monitoring were used. The ion mass spectrum （m/z） of 209, 321, 677 and 823 were selected to quantify panaxsaponin Rg1, icariin, psoralen and isopsoralen, respectively, with lorazepam as an internal standard. Results：The liner range of the calibration curves for panaxsaponin Rg1, icariin, psoralen and isopsoralen were 2.02-12.12, 2.0-12.0, 0.53-1.86, 0.4-1.4 μg·mL^-1 respectively. The contents of panaxsaponin Rg1, icariin, psoralen and isopsoralen per Hongzhu Callrhinus pill were（232.6±0.64）μg,（669.0±14.51）μg,（564±34.71）μg and （428±20.17）μg. Conclusion：The established method is convenient, rapid and accurate, which can be used to determine four components in Hongzhu Callrhinus pills to control its qualities, or to investigate its pharmacokinetic properties in human or animals.

关 键 词：海狗丸 高效液相色谱-质谱 人参皂苷RG1 淫羊藿苷 补骨脂素 异补骨脂素 

分 类 号：R917[医药卫生—药物分析学]