Online restricted-access material combined with high-performance liquid chromatography and tandem mass spectrometry for the simultaneous determination of vanillin and its vanillic acid metabolite in human plasma
Online restricted-access material combined with high-performance liquid chromatography and tandem mass spectrometry for the simultaneous determination of vanillin and its vanillic acid metabolite in human plasma
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DOI：
10.1002/jssc.201600466
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发表时间：
2016-09-01
影响因子：
3.1
通讯作者：
Qi, Jin-long
中科院分区：
文献类型：
--
作者：
Li, De-qiang;Zhang, Zhi-qing;Qi, Jin-long
建立了一种自动化在线固相萃取-高效液相色谱-串联质谱联用技术，用于人血浆中香草醛及其香草酸代谢物的同时定量分析。用含有内标物的甲醇沉淀蛋白质后，将血浆样品的上清液注射到系统中，内源性大分子被冲洗出来，目标分析物被捕获并富集在吸附剂上，从而使样品复杂性和离子抑制效应最小化。香草醛和香草酸的线性范围分别为5-1000 ng/mL和10-5000 ng/mL，测定系数>0.999。香草醛和香草酸的定量下限分别为5.0和10.0 ng/mL。以相对标准偏差表示的批内和批间精密度分别为2.6- 8.6%和3.2- 10.2%，以相对误差表示的准确度范围为-6.1至7.3%。分析物的提取回收率在89.5%和97.4%之间。任何分析物浓度均无显著基质效应。该方法灵敏度高、重复性好、准确度高，可用于人血浆中香草醛及其香草酸代谢物的定量测定。
An automated online solid-phase extraction with restricted-access material combined with high-performance liquid chromatography and tandem mass spectrometry was developed and validated for the simultaneous quantification of vanillin and its vanillic acid metabolite in human plasma. After protein precipitation by methanol, which contained the internal standards, the supernatant of plasma samples was injected to the system, the endogenous large molecules were flushed out, and target analytes were trapped and enriched on the adsorbent, resulting in a minimization of sample complexity and ion suppression effects. Calibration curves were linear over the concentrations of 5-1000 ng/mL for vanillin and 10-5000 ng/mL for vanillic acid with a coefficient of determination >0.999 for the determined compounds. The lower limits of quantification of vanillin and vanillic acid were 5.0 and 10.0 ng/mL, respectively. The intra-and inter-run precisions expressed as the relative standard deviation were 2.6-8.6 and 3.2-10.2%, respectively, and the accuracies expressed as the relative error were in the range of -6.1 to 7.3%. Extraction recoveries of analytes were between 89.5 and 97.4%. There was no notable matrix effect for any analyte concentration. The developed method was proved to be sensitive, repeatable, and accurate for the quantification of vanillin and its vanillic acid metabolite in human plasma.