在线固相萃取-高效液相色谱-电感耦合等离子体质谱联用同时预富集和定量分析海水中的超痕量锡和铅形态
Simultaneous preconcentration and quantification of ultra-trace tin and lead species in seawater by online SPE coupled with HPLC-ICP-MS.
作者信息
Guo Feng, Zeng Pingxiu, Liu Jinhua, Hu Hongmei, Zhu Wenbin, Wang Yuanchao, Cheng Heyong
机构信息
College of Material, Chemistry and Chemical Engineering, Key Laboratory of Organosilicon Chemistry and Material Technology, Ministry of Education, Hangzhou Normal University, Hangzhou, 311121, Zhejiang, China.
Key Laboratory of Sustainable Utilization of Technology Research for Fisheries Resources of Zhejiang Province, Zhejiang Marine Fisheries Research Institute, Zhoushan, 316021, China.
出版信息
Anal Chim Acta. 2024 Mar 15;1294:342294. doi: 10.1016/j.aca.2024.342294. Epub 2024 Jan 27.
BACKGROUND
Tin and lead contamination is a global threat to marine ecosystems considering their species-specific toxicity, bioavailability and mobility. Hence simultaneous measurement of multiple tin and lead compounds at μg L to pg L levels in environmental water is always an indispensable but challengeable task. High performance liquid chromatography coupled with inductively coupled plasma mass spectrometry (HPLC-ICP-MS) is one of the most widely used choices for this purpose because of good sensitivity, strong separation power and good compatibility. Previous HPLC-ICP-MS methods based on a single elemental speciation strategy are low-efficiency and sensitivity-insufficient for a large set of unstable samples and interaction of multiple metal(loid)s down to ng L levels.
RESULTS
In this study, we developed a sensitive, efficient and environment-friendly analytical method for accurate quantification of inorganic and organic species of tin and lead simultaneously based on HPLC-ICP-MS with online integration of solid phase extraction (SPE). By using graphene oxide modified silica conditioned with 1 mM benzoic acid to enrich tin and lead species from 10 mL sample, detection limits were improved to 2-8 pg per liter due to satisfactory enrichment factors (522-2848 folds). The SPE-HPLC-ICP-MS method was applicable to quantification of ultra-trace tin and lead species at pg L levels in uncontaminated seawater. Tributyltin was the only tin species detected at subnanograms per liter levels while Pb(II) was the only lead species detected at several nanograms per liter in thirteen coastal seawater samples collected in Hangzhou Bay, indicating light contamination of tin and lead.
SIGNIFICANCE
Overall, the proposed SPE-HPLC-ICP-MS method is highly sensitive, efficient and environment-friendly that are fairly suitable to routine speciation analysis of tin and lead in environmental, food, and biological samples.
背景
考虑到锡和铅的物种特异性毒性、生物有效性和迁移性，它们的污染是对海洋生态系统的全球威胁。因此，同时测定环境水中微克每升至皮克每升水平的多种锡和铅化合物一直是一项不可或缺但具有挑战性的任务。高效液相色谱与电感耦合等离子体质谱联用（HPLC-ICP-MS）由于灵敏度高、分离能力强和兼容性好，是为此目的最广泛使用的选择之一。以前基于单一元素形态分析策略的HPLC-ICP-MS方法效率低，对于大量不稳定样品以及低至纳克每升水平的多种金属（类金属）相互作用，灵敏度不足。
结果
在本研究中，我们基于HPLC-ICP-MS并在线集成固相萃取（SPE），开发了一种灵敏、高效且环境友好的分析方法，用于同时准确量化锡和铅的无机和有机形态。通过使用用1 mM苯甲酸调节的氧化石墨烯修饰硅胶从10 mL样品中富集锡和铅形态，由于令人满意的富集因子（522 - 2848倍），检测限提高到每升2 - 8皮克。SPE-HPLC-ICP-MS方法适用于量化未受污染海水中皮克每升水平的超痕量锡和铅形态。在杭州湾采集的13个沿海海水样品中，三丁基锡是唯一在每升亚纳克水平检测到的锡形态，而Pb(II)是唯一在每升几纳克水平检测到的铅形态，表明锡和铅的污染较轻。
意义
总体而言，所提出的SPE-HPLC-ICP-MS方法高度灵敏、高效且环境友好，非常适合环境、食品和生物样品中锡和铅的常规形态分析。
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