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高效液相色谱-原子荧光光谱法联用固相萃取法测定水中痕量汞形态分析。

Sensitive Mercury Speciation Analysis in Water by High-Performance Liquid Chromatography-Atomic Fluorescence Spectrometry Coupling with Solid-Phase Extraction.

机构信息

Hunan Provincial Center for Disease Control and Prevention, Changsha, 410005, China.

出版信息

Anal Sci. 2021 Sep 10;37(9):1235-1240. doi: 10.2116/analsci.20P398. Epub 2021 Jan 29.

DOI:10.2116/analsci.20P398
PMID:33518585
Abstract

An efficient method based on high-performance liquid chromatography coupled with atomic fluorescence spectrometry (HPLC-AFS) was successfully developed for the simultaneous determination of four mercury species including Hg, methylmercury (MeHg), ethylmercury (EtHg), and phenylmercury (PhHg) in water. Samples were enriched and cleaned up with a solid-phase extraction (SPE) pretreatment using a thiol cartridge. Some key parameters including the selection of a SPE cartridge, eluent type, eluent volume, and interference factors were systematically investigated. Chromatographic separation was achieved on a C column using a mobile phase consisting of methanol and 60 mmol L ammonium acetate with 10 mmol L L-cysteine by gradient elution. Under the optimized conditions, good linearity (r ≥ 0.9991) was observed between 0.20 to 10.0 μg L. The limits of detection were in the range of 0.001 - 0.002 μg L. High recoveries (87.2 to 111%) and good reproducibility (1.1 - 6.5%) were obtained. Such a method is sensitive, selective and accurate, which can be applied to the quantification of mercury species in water samples.

摘要

建立了一种高效液相色谱-原子荧光光谱法(HPLC-AFS)同时测定水中四种汞形态(Hg、甲基汞(MeHg)、乙基汞(EtHg)和苯基汞(PhHg))的方法。样品经巯基固相萃取(SPE)预处理进行富集和净化。系统考察了SPE 小柱的选择、洗脱液类型、洗脱液体积和干扰因素等关键参数。采用甲醇和 60mmol/L 乙酸铵溶液(含 10mmol/L L-半胱氨酸)作为流动相,在 C 柱上进行梯度洗脱,实现了色谱分离。在优化条件下,0.20-10.0μg/L 范围内线性良好(r≥0.9991)。检出限在 0.001-0.002μg/L 范围内。该方法灵敏度高、选择性好、准确度高,可用于水样中汞形态的定量分析。

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