通过液相色谱-串联质谱法对血浆磷脂进行系统评估，以可靠且精确地测定决奈达隆和去丁基决奈达隆。
Systematic evaluation of plasma phospholipids for reliable and precise determination of dronedarone and desbutyldronedarone by LC-MS/MS.
作者信息
Parekh Jignesh M, Sanyal Mallika, Yadav Manish, Shrivastav Pranav S
机构信息
Chemistry Department, Kadi Sarva Vishwavidyalaya, Gujarat, India.
出版信息
Bioanalysis. 2014;6(19):2635-50. doi: 10.4155/bio.14.123.
BACKGROUND
The objective of the present work was to minimize or eliminate the matrix effect due to plasma phospholipids as observed during sample preparation for accurate determination of dronedarone and its active metabolite, desbutyldronedarone by LC-ESI-MS/MS.
RESULTS
The extraction recovery and matrix factors ranged from 93.27 to 95.14% and 0.99 to 1.02, respectively, for both the analytes. A linear concentration range of 0.10 to 150 ng/ml was established for both the analytes. The analytes were efficiently resolved (R(s) 2.37) on Kromasil(®) (AkzoNobel, Bohus, Sweden) C18 column within 3.0 min. The assay reproducibility was determined by reanalysis of 72 incurred samples with % change within ± 10%.
CONCLUSION
The optimized solid-phase extraction provided cleaner extracts with reduced matrix effect from plasma phospholipids compared with protein precipitation and liquid-liquid extraction.
背景
本研究的目的是在通过液相色谱-电喷雾串联质谱法（LC-ESI-MS/MS）准确测定决奈达隆及其活性代谢物去丁基决奈达隆的样品制备过程中，尽量减少或消除血浆磷脂引起的基质效应。
结果
两种分析物的萃取回收率和基质因子分别为93.27%至95.14%和0.99至1.02。两种分析物均建立了0.10至150 ng/ml的线性浓度范围。在Kromasil®（阿克苏诺贝尔公司，瑞典博胡斯）C18柱上，两种分析物在3.0分钟内有效分离（R(s) 2.37）。通过对72个实际样品进行重新分析来确定分析方法的重现性，变化百分比在±10%以内。
结论
与蛋白沉淀和液液萃取相比，优化后的固相萃取提供了更纯净的提取物，减少了血浆磷脂的基质效应。
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