Ultra-performance liquid chromatography-tandem mass spectrometric method for the determination of strychnine and brucine in mice plasma

Ultra-performance liquid chromatography-tandem mass spectrometric method for the determination of strychnine and brucine in mice plasma
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超高效液相色谱-串联质谱法测定小鼠血浆中士的宁和马钱子碱

DOI:
10.1016/j.jchromb.2011.07.033
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发表时间:
2011-09-15
影响因子:
3
通讯作者:
Lei, Yanqing
Lei, Yanqing
中科院分区:
医学3区
文献类型:
--
作者:
Liu, Yanwen;Zhu, Ronghua;Lei, Yanqing

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建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)测定小鼠血浆中士的宁和马钱子碱的方法。采用1.7 μ m BEH C-18色谱柱(50 mm x 2.1 mm)进行UPLC分离,移动的流动相由甲醇:0.1%甲酸(25:75,v/v)组成,因此可为分析物和内标物提供高效率、高分离度和良好的峰形。士的宁和马钱子碱分别在2.48-496.4 ng/ml和2.64-528 ng/ml的范围内验证了该方法。士的宁和马钱子碱的日内和日间准确度分别为95.0%~ 107.9%和93.4%~ 103.3%,精密度均在13.8%以内。两种生物碱的提取回收率均大于81.9%。由于样品制备过程简单,运行时间短,
A selective, simple and efficient method-ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for determination of two toxic alkaloids, namely strychnine and brucine in mice plasma. The UPLC separation was carried out using a 1.7 mu m BEH C-18 column (50 mm x 2.1 mm) with a mobile phase consisting of methanol:0.1% formic acid (25:75, v/v), hence providing high efficiency, high resolution and excellent peak shape for the analytes and internal standard. The method was validated over the range of 2.48-496.4 ng/ml for strychnine and 2.64-528 ng/ml for brucine, respectively. Intra- and inter-day accuracy ranged from 95.0% to 107.9% for strychnine, 93.4% to 103.3% for brucine, and the precisions were within 13.8%. The extraction recoveries of both the two alkaloids exceed 81.9%. With a simple and minor sample preparation procedure and short run-time (