An interface for sensitive analysis of monoamine neurotransmitters by ion-pair chromatography-electrospray ionization-mass spectrometry with continuous online elimination of ion-pair reagents.
An interface for sensitive analysis of monoamine neurotransmitters by ion-pair chromatography-electrospray ionization-mass spectrometry with continuous online elimination of ion-pair reagents.
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DOI：
10.1021/ac401396j
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发表时间：
2013-07-16
影响因子：
7.4
通讯作者：
Zhou, Feimeng
中科院分区：
文献类型：
--
作者：
Shi, Shuyun;Zhao, Binqing;Yagnik, Gargey;Zhou, Feimeng
离子对色谱（IPC）与电喷雾电离质谱（ESI-MS）在线耦合的一个挑战是，流动相中的非挥发性离子对试剂（如胺用硫酸烷基或羧酸用四丁基铵）会抑制气相中的ESI-MS信号，并且它们的积累会堵塞MS采样界面。因此，IPC-ESI-MS要么使用挥发性离子对试剂进行，这可能会降低分析物的分离效率，要么使用下游离子交换柱去除流动相中的离子对试剂。在后一种方法中，离子交换柱的容量有限，需要频繁的离线柱再生，这影响了分离吞吐量，并禁止进行长时间分离。双阀，双离子交换柱接口的IPC-ESI-MS是专为不间断分离和同时柱再生。离子阱质谱检测单胺类神经递质，多巴胺和DA的检出限为0.03 μM， 5-羟色胺和5-HT的检出限为0.01 μM。当结合使用专用色谱柱或样品预浓缩时，这些值低于具有相似灵敏度的离子阱质谱所获得的值。反复再生离子交换柱的重现性很好（RSD = 4-6%），可延长时间（RSD < 6%， 6天）。我们分析了大鼠睾丸提取物中的DA和5-羟色胺，我们的数据表明，组织和离子对试剂固有的干扰已被成功消除。这个简单的界面应该很容易适用于复杂样品介质中其他类型极性化合物的分离和质谱分析。
A challenge in coupling ion-pair chromatography (IPC) on-line with electrospray ionization-mass spectrometry (ESI-MS) is that the nonvolatile ion-pair reagent (e.g., alkyl sulfate for amines or tetrabutylammonium for carboxylic acids) in the mobile phase suppresses the ESI-MS signals in the gas phase and their accumulation can clog the MS sampling interface. Consequently, IPC–ESI-MS is conducted either with a volatile ion-pair reagent, which could compromise the analyte separation efficiency, or with a downstream ion-exchange column to rid the ion-pair reagents of the mobile phase. In the latter approach, the limited capacity of ion-exchange columns requires frequent off-line column regeneration, which affects the separation throughput and prohibits long separations from being performed. A dual-valve, dual-ion exchange column interface of IPC–ESI-MS is designed for undisrupted separations and simultaneous column regeneration. Owing to the efficacy in removing the ion-pair reagent, the detection of eluents of monoamine neurotransmitters by an ion trap MS results in the limits of detection of 0.03 μM for dopamine or DA and 0.01 μM for 5-hydroxytryptamine or 5-HT. These values are lower than those obtained with ion trap MS of similar sensitivity when combined with the use of specialized chromatographic columns or sample preconcentration. Excellent reproducibility was attained with repeatedly regenerated ion-exchange columns (RSD = 4–6%) for an extended period of time (RSD < 6% for six days). DA and 5-HT in rat straital extracts were analyzed and our data demonstrate that interferences inherent in the tissues and the ion-pair reagent have been successfully eliminated. This simple interface should be readily amenable to the separation and MS analysis of other types of polar compounds in complex sample media.
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影响因子：
7.4
作者：
Ji, Chengjie;Li, Wenlin;Lepsy, Christopher
通讯作者：
Lepsy, Christopher
影响因子：
4.7
作者：
ROWLETT, JK;MATTINGLY, BA;BARDO, MT
通讯作者：
BARDO, MT
影响因子：
4.1
作者：
VREEKEN, RJ;GHIJSEN, RT;BRINKMAN, UAT
通讯作者：
BRINKMAN, UAT
影响因子：
4.1
作者：
Forngren, BH;Samskog, J;Långström, B
通讯作者：
Långström, B
影响因子：
7.4
作者：
Gangl, ET;Annan, M;Vouros, P
通讯作者：
Vouros, P