色谱

色谱 ›› 2013, Vol. 31 ›› Issue (9): 894-897.DOI: 10.3724/SP.J.1123.2013.01051

• 技术与应用 • 上一篇    下一篇

适用于质谱分析的在线固相萃取除盐方法

陈静1,2, 刘召金3, 戴振宇2, 安保超2, 许群2, 张祥民1   

  1. 1. 复旦大学化学系, 上海 200433;
    2. 赛默飞世尔科技中国有限公司, 上海 201203;
    3. 山东省邹城市食品质量检验中心, 山东 邹城 273500
  • 收稿日期:2013-01-30 修回日期:2013-03-08 出版日期:2013-09-28 发布日期:2013-09-02
  • 通讯作者: 许群
  • 基金资助:

    国家自然科学基金项目(21175026).

On-line solid phase extraction for desalting coupled with mass spectrometric analysis

CHEN Jing1,2, LIU Zhaojin3, DAI Zhenyu2, AN Baochao2, XU Qun2, ZHANG Xiangmin1   

  1. 1. Department of Chemistry, Fudan University, Shanghai 200433, China;
    2. ThermoFisher Scientific China, Shanghai 201203, China;
    3. Zoucheng Food Quality Inspection Center of Shandong Province, Zoucheng 273500, China
  • Received:2013-01-30 Revised:2013-03-08 Online:2013-09-28 Published:2013-09-02

PDF

343

被引次数

6

摘要：

建立了一个简单、快速、有效的适用于质谱或液相色谱-质谱联用的在线固相萃取(SPE)高通量除盐方法。方法分为单柱和双柱模式,借助于包含双梯度泵(上样泵/分析泵)、自动进样器和配有十通切换阀的柱温箱的高效液相色谱系统,完成样品的自动化在线除盐。单柱模式通过上样泵实现在SPE柱上进样和除盐,被分析物则保留在SPE柱上;除盐完成后,通过阀切换利用分析泵洗脱富集在SPE柱上的被分析物。双柱模式则在单柱模式基础上增加了1根SPE柱,在色谱管理软件控制下2根SPE柱轮流工作,高效率完成样品的在线除盐。该方法在结合质谱分析蛋白质、多肽等领域具有较好的应用前景。

关键词: 除盐, 阀切换, 固相萃取, 双梯度高效液相色谱系统, 在线

Abstract:

The work shown here describes a simple, fast and effective on-line solid phase extraction (on-line SPE) method for facilitative high-throughput sample desalting before the detection of mass spectrometry(MS)or liquid chromatography-mass spectrometry(LC-MS). This method includes single SPE column mode and dual SPE column mode. It accomplishes the on-line desalting with an Ultimate 3000 HPLC system equipped with a dual pump system (loading pump/analytical pump), an autosampler, a column oven equipped with a 2p-10p valve, controlled by a chromatography data system. In the single SPE column mode, sample loading and desalting were performed on the SPE column using the loading pump. The analytes were retained on the SPE column, and the salt in the sample solution was flushed out of the SPE column. After desalting, the retained analytes were eluted from the SPE column with the analytical pump. In the dual SPE column mode, two same SPE columns were used. Firstly, the sample loading and desalting were performed on the SPE column 1. The analytes were retained and the salt was flushed out. After desalting on the SPE column 1, the sample loading and desalting were performed on the SPE column 2. Meanwhile, the retained analytes were eluted from the SPE column 1 with the analytical pump. As both of the processes on the SPE columns 1 and 2 described above completed, the sample loading and desalting on the SPE column 1, and the elution of the analytes from the SPE column 2 started again. As the SPE columns 1 and 2 worked in turn, the on-line SPE desalting system was efficient. The eluted analytes from the SPE columns may be determined by MS directly, or separated on the analytical column and then determined by MS/UV.

Key words: desalt, dual-gradient high performance liquid chromatography (HPLC), on-line, solid phase extraction (SPE), valve-switching

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