LC-MS/MS技术同时测定滋心阴口服液中6种化学成分  

Simultaneous determination of six components in Zixinyin Oral Liquid by LC-MS/MS

作　　者：乔湜[1] 石蕊[1] 蒋午峻[1] 卢树杰 王巧[1] 张兰桐[1] 

机构地区：[1]河北医科大学药学院药物分析教研室,河北石家庄050017 [2]河北省中药注射剂工程技术研究中心,河北石家庄051430

出　　处：《中成药》2011年第3期456-460,共5页Chinese Traditional Patent Medicine

摘　　要：目的:建立HPLC-ESI-MS方法同时测定滋心阴口服液(北沙参、赤芍、麦冬、三七)中6种化学成分。方法:采用多反应监测(MRM)模式同时监测4种香豆素类和2种苷类成分。ESI源,正、负离子同时检测,源喷射电压分别为5 500 V和-4 500 V,离子源温度为650℃。6种被测成分的监测离子对分别为479.1/121.0(芍药内酯苷)、525.2/449.1(芍药苷)、217.1/202.1(花椒毒素)、187.2/131.1(补骨脂素)、247.1/217.0(异茴芹内酯)和217.1/202.1(佛手柑内酯)。色谱柱为Agilent Zorbax SB-C18柱,流动相为甲醇-0.1‰甲酸,梯度洗脱,分析时间7.5 min。采用所建立的方法对4批滋心阴口服液进行了测定。结果:6种化学成分的峰面积和浓度在测定浓度范围内均具有良好的线性关系,平均加样回收率为91.7%～108.7%,精密度RSD为1.1%～3.0%。结论:本法简便、快速、灵敏度高、专属性好,可用于滋心阴口服液中芍药内酯苷、芍药苷、花椒毒素、补骨脂素、异茴芹内酯和佛手柑内酯的含量测定。除芍药苷外,其它5种成分均为滋心阴口服液中首次测定。AIM： To develop a liquid chromatography-tandem mass spectrometry （LC-MS/MS） method for simultaneously analysing six components in Zixinyin Oral Liquid （ Glehniae Radix, Paeoniae Radix rubra, Ophiopogonis Radix, Notoginseng Radix et Rhizoma）. METHODS： Multiple reaction monitoring （MRM） scan mode was used for quantification. The mass spectrometer was performed using eleetrospray ionization source in positive and negative mode simultaneously. The ion spray voltage was set to 5 500 V and -4 500 V, respectively. The turbo spray temperature was maintained at 650 ℃. The precursor-to-product ion pairs of six analytes were 479.1/121.0 for albiflorin, 525.2/449. 1 for paeoniflorin, 217. 1/202. 1 for xanthotoxin, 187.2/131.1 for psoralen, 247.1/ 217.0 for isopimpinellin and 217.1/202.1 for bergapten, respectively. The six constituents were separated within 7.5 min on an Agilent Zorbax SB-C18 column （150 mm ×4.6 mm, 5 μm） using a mobile phase consisted of methanol and 0.1‰ formic acid in water with gradient elution. RESULTS： The average recovery ranged from 91.7% to 108.7%, and the precision in terms of RSD was in the range of 1.1% -3.0%. The linear relationship, linearity range, precision and stability of the method were good for the six components. CONCLUSION： The method is sensitive and suitable for simultaneous determination of six constituents in Zixinyin Oral Liquid. Among these constituents, albiflorin, xanthotoxin, bergapten, isopimpinellin and psoralen are quantified for the first time.

关 键 词：HPLC-MS 滋心阴口服液 芍药内酯苷 芍药苷 花椒毒素 补骨脂素 异茴芹内酯 佛手柑内酯 

分 类 号：R927.2[医药卫生—药学]