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采用微径反相液相色谱-超声喷雾电离质谱法测定水样中的氯酸根、高氯酸根和溴酸根阴离子。

Determination of chlorate, perchlorate and bromate anions in water samples by microbore reversed-phase liquid chromatography coupled to sonic-spray ionization mass spectrometry.

作者信息

Mavroudakis Leonidas, Mavrakis Emmanouil, Kouvarakis Antonis, Pergantis Spiros A

机构信息

Environmental Chemical Processes Laboratory, Department of Chemistry, University of Crete, Voutes Campus, Heraklion, 71003, Greece.

出版信息

Rapid Commun Mass Spectrom. 2017 Jun 15;31(11):911-918. doi: 10.1002/rcm.7866.

DOI:10.1002/rcm.7866
PMID:28370581
Abstract

RATIONALE

Sonic-spray ionization mass spectrometry (SSI-MS) has recently been shown to provide similar mass spectra to those generated by electrospray ionization mass spectrometry for a wide range of compounds, i.e. from small inorganic species to peptides, proteins and numerous other biomolecules. However, limited information about this new ionization technique, such as sensitivity, limit of detection and quantification accuracy, has been reported. In particular, its coupling to liquid chromatography needs further development and assessment, along with the introduction of a broad range of applications.

METHODS

A high-efficiency glass pneumatic nebulizer, used for decades for sample introduction in atomic spectrometry, was used for the SSI-MS analysis of chlorate (ClO ), perchlorate (ClO ) and bromate (BrO ) anions, following their separation using reversed-phase microbore high-performance liquid chromatography and tandem mass spectrometry (MS/MS) operated in selected reaction monitoring mode.

RESULTS

The developed and optimized microbore HPLC/SSI-MS/MS technique exhibited low limits of detection: 5.3 ng L for chlorate, 10 ng L for perchlorate and 33.7 ng L for bromate, and provided reliable and accurate measurements of chlorate concentrations in water samples as demonstrated when comparing it with Ion Chromatography-Conductivity Detection (IC-CD), the benchmark technique for ion quantitation.

CONCLUSIONS

This is the first time that the use of HPLC/SSI-MS/MS has been reported for the detection and quantitation of chlorate, perchlorate and bromate in water samples. In addition, the exceptionally low LODs achieved using SSI render the technique competitive with the established and dominating electrospray ionization technique. Here, we have demonstrated that a commercially available high-efficiency glass pneumatic nebulizer can also be used, without any further modification, as an efficient gas-phase ion source. Copyright © 2017 John Wiley & Sons, Ltd.

摘要

原理

最近研究表明,对于从无机小分子到肽、蛋白质及众多其他生物分子等多种化合物,声喷雾电离质谱(SSI-MS)所提供的质谱图与电喷雾电离质谱生成的质谱图相似。然而,关于这种新电离技术的信息有限,如灵敏度、检测限和定量准确性等方面的报道较少。特别是,它与液相色谱的联用需要进一步发展和评估,同时还需引入广泛的应用。

方法

一个用于原子光谱分析中样品引入且已使用数十年的高效玻璃气动雾化器,被用于对氯酸盐(ClO )、高氯酸盐(ClO )和溴酸盐(BrO )阴离子进行SSI-MS分析,这些阴离子是在反相微径高效液相色谱分离后,采用选择反应监测模式运行的串联质谱(MS/MS)进行分析的。

结果

所开发和优化的微径HPLC/SSI-MS/MS技术展现出低检测限:氯酸盐为5.3 ng/L,高氯酸盐为10 ng/L,溴酸盐为33.7 ng/L,并且在与离子色谱 - 电导检测(IC-CD)(离子定量的基准技术)比较时,能可靠、准确地测量水样中的氯酸盐浓度。

结论

这是首次报道使用HPLC/SSI-MS/MS检测和定量水样中的氯酸盐、高氯酸盐和溴酸盐。此外,使用SSI实现的极低检测限使该技术与已确立且占主导地位的电喷雾电离技术具有竞争力。在此,我们证明了一种市售的高效玻璃气动雾化器无需任何进一步改装,也可作为一种高效的气相离子源使用。版权所有© 2017约翰威立父子有限公司。

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