Interfacing nanoliter liquid chromatography and inductively coupled plasma mass spectrometry with an in-column high-pressure nebulizer for mercury speciation
Interfacing nanoliter liquid chromatography and inductively coupled plasma mass spectrometry with an in-column high-pressure nebulizer for mercury speciation
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将纳升液相色谱法和电感耦合等离子体质谱仪与柱内高压雾化器连接进行汞形态分析
DOI：
10.1016/j.chroma.2018.09.023
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发表时间：
2018
影响因子：
4.1
通讯作者：
Jinhua Liu
中科院分区：
文献类型：
--
作者：
Heyong Cheng;Wenwen Zhang;Yuanchao Wang;Jinhua Liu
临床、生物和法医学领域中微量样品的金属形态分析对于阐明金属的毒性、迁移性和代谢行为具有重要意义。这种分析可以通过纳升高效液相色谱（nanoHPLC）与电感耦合等离子体质谱（ICP-MS）联用来实现。在这项工作中，开发了一种柱内高压雾化器 (ICHPN)，以提高无鞘 nanoHPLC-ICP-MS 耦合的灵敏度和分离效率。 ICHPN 由两个具有锥形尖端的同心熔融石英毛细管组成，通过 PEEK 三通连接，其中基于梯形效应将尺寸为 5μm 的 C18 二氧化硅颗粒填充在锥形内部毛细管中。 ICHPN 将加热的单通道雾化室与尾吹气相结合，能够独立优化雾化效率和传输效率。 ICHPN 在纳流速率下具有高灵敏度、低检测限和良好的精度。与商业雾化器相比，ICHPN 制造简单、快速、可重复且廉价。通过实施 ICHPN，我们在 8.0 分钟内实现了四种汞形态的快速分离，即 Hg2+ 和氯化甲基、乙基和苯基汞，并具有良好的分辨率 (2.0–13.9)。对于 50μgL−1 标准溶液，检测限为 0.044-0.13μgL−1，峰高和面积精度为 1.5% 至 3.5%。山羊血液认证参考材料 (SRM 955c) 中汞形态的测定值与认证值之间的良好一致性以及良好的回收率 (93–101%) 验证了该方法的准确性。
Metal speciation analysis of microsamples in the clinical, biological and forensic fields is important for elucidating the metals’ toxicity, mobility and metabolic behaviors of metals. Such analysis may be achieved by nanoliter high-performance liquid chromatography (nanoHPLC) hyphenated with inductively coupled plasma mass spectrometry (ICP-MS). In this work, an in-column high-pressure nebulizer (ICHPN) was developed to enhance the sensitivity and the separation efficiency of the sheathless nanoHPLC-ICP-MS coupling. The ICHPN consists of two concentric fused-silica capillaries with tapered tips connectedviaa PEEK tee, where C18silica particles with a size of 5 μm were packed in the tapered inner capillary based on the keystone effect. Combining a heated single pass spray chamber with a makeup gas, the ICHPN was capable of independently optimizing the nebulization efficiency and the transport efficiency. The ICHPN offered high sensitivities, low detection limits and good precision at nanoflow rates. Compared with commercial nebulizers, the ICHPN fabrication was simple, rapid, reproducible and inexpensive. By implementing the ICHPN, we achieved rapid separation of four mercury species,i.e., Hg2+and methyl-, ethyl- and phenylmercuric chloride, within 8.0 min with good resolution (2.0–13.9). Detection limits of 0.044-0.13 μg L−1were obtained with precisions of peak heights and areas ranging from 1.5 to 3.5% for a 50 μg L−1standard solution. Good agreement between the determined and certified values of mercury species in a certified reference material of caprine blood (SRM 955c) together with good recoveries (93–101%) validated the accuracy of the method.