A four-column parallel chromatography system for isocratic or gradient LC/MS analyses.
A four-column parallel chromatography system for isocratic or gradient LC/MS analyses.
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用于等度或梯度 LC/MS 分析的四柱平行色谱系统。
DOI：
10.1021/ac0006876
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发表时间：
2001
影响因子：
7.4
通讯作者：
J. Henion
中科院分区：
文献类型：
--
作者：
C. V. Van Pelt;T. Corso;G. Schultz;S. Lowes;J. Henion
提出了一种用于药代动力学分析和类似定量应用的平行液相色谱/串联质谱（LC/MS/MS）分析的新方法。适度的修改使传统的LC/MS系统能够并行分析样品。这些修改涉及简单的三个阀门和四个LC柱到一个传统的系统组成的一个二元LC泵系统，一个自动进样器，和一个质谱仪。通过交错进样到四个色谱柱上来提高样品通量，使质谱仪能够连续分析感兴趣的色谱窗口。使用这种方法，优化的运行时间略大于所需峰的宽度之和。该平行色谱装置可在梯度和等度LC条件下操作。为了证明该系统的实用性，使用梯度洗脱色谱条件分析了阿托伐他汀、其五种代谢产物及其氘代内标物（IS）。提供了来自提取加标人血浆的标准品和质控（QC）样品的研究前试验评价（PSAE）托盘的结果。QC样品的相对标准偏差和准确度分别不超过8.1%和9.6%，完全在制药行业的验收标准范围内。对于该特定分析，平行色谱系统将总运行时间从4.5分钟减少到1.65分钟，因此，与常规LC/MS/MS分析方法相比，总通量增加了2.7倍。
A novel approach to parallel liquid chromatography/ tandem mass spectrometry (LC/MS/MS) analyses for pharmacokinetic assays and for similar quantitative applications is presented. Modest modifications render a conventional LC/MS system capable of analyzing samples in parallel. These modifications involve the simple incorporation of three valves and four LC columns into a conventional system composed of one binary LC pumping system, one autosampler, and one mass spectrometer. An increase in sample throughput is achieved by staggering injections onto the four columns, allowing the mass spectrometer to continuously analyze the chromatographic window of interest Using this approach, the optimized run time is slightly greater than the sum of the widths of the desired peaks. This parallel chromatography unit can operate under both gradient and isocratic LC conditions. To demonstrate the utility of the system, atorvastatin, five of its metabolites, and their deuterated internal standards (IS) were analyzed using gradient elution chromatography conditions. The results from a prestudy assay evaluation (PSAE) tray of standards and quality control (QC) samples from extracted spiked human plasma are presented. The relative standard deviation and the accuracy of the QC samples did not exceed 8.1% and 9.6%, respectively, which is well within the acceptance criteria of the pharmaceutical industry. For this particular analysis, the parallel chromatography system decreased the overall run time from 4.5 to 1.65 min and, therefore, increased the overall throughput by a factor of 2.7 in comparison to a conventional LC/MS/MS analytical method.