Nonvolatile salt-free stabilizer for the quantification of polar imipenem and cilastatin in human plasma using hydrophilic interaction chromatography/quadrupole mass spectrometry with contamination sensitive off-axis electrospray.
Nonvolatile salt-free stabilizer for the quantification of polar imipenem and cilastatin in human plasma using hydrophilic interaction chromatography/quadrupole mass spectrometry with contamination sensitive off-axis electrospray.
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DOI：
10.1002/jms.3240
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发表时间：
2013-08
影响因子：
2.3
通讯作者：
Hickerson, William L.
中科院分区：
文献类型：
--
作者：
Hu, Zhe-Yi;Boucher, Bradley A.;Laizure, S. Casey;Herring, Vanessa L.;Parker, Robert B.;Hickerson, William L.
关键词：
建立了亚胺培南(IMP)和西司他丁(CIL)的亲水作用色谱-质谱仪(HILIC-MS)分析方法。这种基于正交电喷雾离子源(ORS)的分析方法利用非挥发性盐(不可去除)来稳定血浆中的IMI。遗憾的是，这种方法不适用于传统的离轴喷雾MS(OAS-MS)，因为非挥发性盐会迅速降低MS的灵敏度。因此，我们的目标是找到一种非挥发性、无盐和离子抑制的方法来稳定和测量血浆中的分析物，使用OAS-MS。用乙腈和甲醇来稳定血浆样品中的分析物。对稳定剂处理样品的回收率、基质效应和稳定性进行了研究。MS信号强度的变化被用来作为检测坚固性的指标。结果表明，用甲醇-乙腈(1：1)混合溶液储存和测定人血浆中IMP和CIL的效果最佳。这种沉淀剂的使用不仅阻止了血浆中分析物的水解，而且还获得了无离子抑制、快速(每个样品120 S)和灵敏的检测方法。使用灵敏度较低的OAS-MS(API3000，柱上4pg)获得的灵敏度远远高于已发表的基于ORS-MS的分析方法(API4000，柱上77pg)。通过其恒定的MS信号强度，证明了该方法的坚固性。综上所述，建立了一种改进的基于HILIC/MS的IMP和CIL检测方法。本文提出的方法为分析生物样品中不稳定的β-内酰胺类抗生素提供了一个简单的解决方案。
A hydrophilic interaction chromatography/mass spectrometry (HILIC-MS)-based assay for imipenem (IMP) and cilastatin (CIL) was recently reported. This orthogonal electrospray ion source-based (ORS) assay utilized nonvolatile salt (unremovable) to stabilize IMI in plasma. Unfortunately, this method was not applicable to conventional MS with off-axis spray (OAS-MS) because MS sensitivity was rapidly deteriorated by the nonvolatile salt. Therefore, we aimed to find a nonvolatile salt- and ion suppression-free approach to stabilize and measure the analytes in plasma using OAS-MS. Acetonitrile and methanol were tested to stabilize the analytes in the plasma samples. The recoveries, matrix effects and stabilities of the analytes in the stabilizer treated samples were studied. The variations in MS signal intensities were used as the indicator of the assay ruggedness. The results show that a mixture of methanol and acetonitrile (1:1) is best for the storage and measurement of IMP and CIL in human plasma. Utilization of this precipitant not only blocked the hydrolysis of the analytes in plasma but also resulted in an ion suppression-free, fast (120 s per sample) and sensitive detection. The sensitivity obtained using the less sensitive OAS-MS (API3000, 4 pg on column) is much greater than that of the published ORS-MS-based assay (API4000, 77 pg on column). The ruggedness of the assay was demonstrated by its constant MS signal intensity. In conclusion, an improved HILIC/MS-based assay for IMP and CIL was established. The approach presented here provides a simple solution to the challenge of analyzing hydrolytically unstable β-lactam antibiotics in biological samples.
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在体外dabigatran et催化代谢的研究中，常规的液相色谱/三极质质谱法代谢物鉴定和半定量估计方法。
影响因子：
4.3
作者：
Hu, Zhe-Yi;Parker, Robert B.;Herring, Vanessa L.;Laizure, S. Casey
通讯作者：
Laizure, S. Casey
影响因子：
6.2
作者：
Fernandez-Torres, R.;Bello-Lopez, M. A.;Jimenez-Sanchez, J. C.
通讯作者：
Jimenez-Sanchez, J. C.
影响因子：
2
作者：
Xu, Yang;Xie, Wei;Woolf, Eric J.
通讯作者：
Woolf, Eric J.
DOI：
10.1016/0378-4347(84)80069-9
发表时间：
1984-01-01
期刊：
JOURNAL OF CHROMATOGRAPHY
影响因子：
--
作者：
GRAVALLESE, DA;MUSSON, DG;BAYNE, WF
通讯作者：
BAYNE, WF
影响因子：
7.4
作者：
Creek, Darren J.;Jankevics, Andris;Burgess, Karl E. V.
通讯作者：
Burgess, Karl E. V.