作者：李艳苹, 王翠翠, 赵剑超, 马明远, 刘小骐, 高艾

作者单位：自然资源部天津海水淡化与综合利用研究所，天津 300192

关键词：液相色谱;氢化物发生-原子荧光光谱;硒;形态;海水;浓盐水

摘要：

采用高效液相色谱-氢化物发生-原子荧光光谱联用技术，建立了海水及浓盐水中有机硒和无机硒形态的测定方法。探讨氢化物发生反应条件、色谱分离条件及样品基体对硒形态测定的影响，并给出最优的分析条件。使用Hamilton PRP-X100分析柱，30 mmol/L（pH 4）的柠檬酸缓冲溶液为流动相进行洗脱。在载流15% HCl、还原剂2.5% KBH₄ + 0.5% KOH、碘化钾0.25% 的反应条件下，8.5 min可完成4种硒形态的分离和测定，方法的分离和测定效果良好。研究表明，在5~200 μg/L范围内，SeCys₂、MeSeCys、SeMet和SeO₄^2– 4种硒形态的线性相关系数均大于0.998，检出限分别为2.40 μg/L、0.50 μg/L、1.97 μg/L和0.53 μg/L。对海水和人工盐水分别进行加标回收率和精密度的试验，测得加标回收率为77.5%~119%，硒形态测定的相对标准偏差为3.5%~12.5%。方法的准确度、精密度高，加标回收效果好，为测定海水及浓盐水中硒形态的高效快速分析方法。

Determination of selenium species in seawater and brine by liquid chromatography-atomic fluorescence spectrometry
LI Yanping, WANG Cuicui, ZHAO Jianchao, MA Mingyuan, LIU Xiaoqi, GAO Ai
The Institute of Seawater Desalination and Multipurpose Utilization, MNR(Tianjin), Tianjin 300192, China
Abstract: A method was developed for the determination of organic selenium and inorganic selenium species in seawater and brine by hyphenated technique of high performance liquid chromatography-hydride generation-atomic fluorescence spectrometry(HPLC-HG-AFS). The effects of hydride generation reaction conditions, chromatographic separation conditions and sample matrix on the determination of selenium species were discussed, and the optimal analysis conditions were given. In this method, Hamilton PRP-X100 was used as the analytical column, and 30 mmol/L citric acid buffer solution (pH 4) was used as the mobile phase for elution. Under the reaction conditions of carrier 15% HCl, reducing agent 2.5% KBH₄ + 0.5% KOH and potassium iodide 0.25%, the separation and determination of four selenium species can be completed within 8.5 min. The separation and determination results of the method are good. In the range of 5 μg/L to 200 μg/L, the linear correlation coefficients of SeCys₂, MeSeCys, SeMet and SeO₄^2– selenium species were all better than 0.998, and the detection limits were found to be 2.40, 0.50, 1.97 and 0.53 μg/L respectively. Tests for recovery and precision were made by addition of standard solutions to the samples of seawater and salt water. The recoveries were in the range of 77.5%-119%，and the precisions were in the range of 3.5%-12.5%. The method has high accuracy, precision and good recovery effect. It is an efficient and rapid method for the determination of selenium species in seawater and brine.
Keywords: liquid chromatography;hydride generation-atomic fluorescence spectrometry;selenium;species;seawater;brine
2022, 48(10):41-45  收稿日期: 2021-03-12;收到修改稿日期: 2021-06-09
基金项目: 中央级公益性科研院所基本科研业务费专项资金项目（K-JBYWF-2017-T14）；天津市重点研发计划资助项目（19YFZCSN01130）
作者简介: 李艳苹（1978-），女，河南开封市人，高级工程师，硕士，主要从事海水、苦咸水及排放水分析
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