超高效液相色谱-质谱/质谱联用法同时测定大鼠血浆中的长春西汀和代谢物阿朴长春胺酸

张丽丽,鲁亚楠,王新涛,秦峰,隋杨,袁悦,熊志立

中国药学杂志 ›› 2013, Vol. 48 ›› Issue (22) : 1954-1958.

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中国药学杂志 ›› 2013, Vol. 48 ›› Issue (22) : 1954-1958. DOI: 10.11669/cpj.2013.22.016
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超高效液相色谱-质谱/质谱联用法同时测定大鼠血浆中的长春西汀和代谢物阿朴长春胺酸

  • 张丽丽,鲁亚楠,王新涛,秦峰,隋杨,袁悦,熊志立*
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Simultaneous Determination of Vinpocetine and Apovincaminic Acid in Rat Plasma by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

  • ZHANG Li-li,LU Ya-nan,WANG Xin-tao,QIN Feng,SUI Yang,YUAN Yue,XIONG Zhi-li*
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摘要

目的 建立超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定血浆中长春西汀(VP)及其代谢物阿朴长春胺酸(AVA)的浓度。方法 血浆样品经HCl酸化后用乙酸乙酯液-液萃取,以非那西汀为内标, 采用ACQUITY UPLC BEH C18柱(2.1 mm×100 mm,1.7 μm)分离,以甲醇-水溶液为流动相进行梯度洗脱,流速为0.2 mL·min-1, 通过电喷雾离子源(ESI),采用多反应监测(MRM)正离子方式检测。结果 长春西汀在0.40~149 ng·mL-1(r=0.994 4),阿朴长春胺酸(AVA)在0.80~298 ng·mL-1(r=0.994 9)内线性良好。准确度(RE%)长春西汀为-5.9%~7.3%、阿朴长春胺酸为-7.9%~ 5.6%,长春西汀的日内和日间精密度(RSD)均小于12.9 %,阿朴长春胺酸的日内和日间精密度(RSD)均小于11.1%。结论 所建立的UPLC-MS/MS专属性好,灵敏度高,操作简便,已成功用于长春西汀片剂在大鼠体内的药物动力学研究。

Abstract

To develop a specific,rapid, and sensitive ultra-performance liquid chromatography-tandem mass spectrometry method for simultaneous determination of vinpocetine (VP) and its metabolite, apovincaminic acid (AVA) , in rat plasma. METHODS The plasma samples were acidified and extracted with ethyl acetate. Phenacetin was used as internal standard (I.S). The separation was performed on a Waters ACQUITY UPLC BEH C18 column(2.1 mm×100 mm,1.7 μm). The mobile phase was composed of methanol-water with gradient elution at the flow rate of 0.20 mL·min-1. The detection was performed on a triple quadrupole tandem mass spectrometer in multiple reaction monitoring mode via electrospray ionization source(ESI)with positive mode. RESULTS The calibration curve was linear in concentration range from 0.40 to 149 ng·mL-1 for vinpocetine and 0.80 to 298 ng·mL-1 for apovincaminic acid. The intra-day and inter-day precision (relative standard deviation) values were within 12.9%,the accuracy (relative error) was from -5.9% to 7.3% for vinpocetine and-7.9% to 5.6% for apovincaminic acid at all quality control levels. CONCLUSION The UPLC-MS/MS method is specific,rapid, sensitive, and is successfully applied to the pharmacokinetic study of VP tables in rat plasma after intragastric administration.

关键词

长春西汀 / 阿朴长春胺酸 / 超高效液相色谱-串联质谱 / 药动学

Key words

vinpocetine(VP) / apovincaminic acid(AVA) / UPLCMS/MS / pharmacokinetics

引用本文

导出引用
张丽丽,鲁亚楠,王新涛,秦峰,隋杨,袁悦,熊志立. 超高效液相色谱-质谱/质谱联用法同时测定大鼠血浆中的长春西汀和代谢物阿朴长春胺酸[J]. 中国药学杂志, 2013, 48(22): 1954-1958 https://doi.org/10.11669/cpj.2013.22.016
ZHANG Li-li,LU Ya-nan,WANG Xin-tao,QIN Feng,SUI Yang,YUAN Yue,XIONG Zhi-li. Simultaneous Determination of Vinpocetine and Apovincaminic Acid in Rat Plasma by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Pharmaceutical Journal, 2013, 48(22): 1954-1958 https://doi.org/10.11669/cpj.2013.22.016
中图分类号: R917   

参考文献

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基金

基金项目:国家自然科学基金资助项目(30873367)

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