Laboratoire de Chimie Analytique Bio-inorganique et Environnement (LCABIE), Institut Pluridisciplinaire de Recherche sur l'Environnement et les Matériaux (IPREM), CNRS UMR 5254, Université de Pau et des Pays de l'Adour, Hélioparc Pau Pyrénées, 2, av. P. Angot, 64053, Pau cedex 9, France.
Anal Bioanal Chem. 2014 Feb;406(4):1253-8. doi: 10.1007/s00216-013-7373-4. Epub 2013 Oct 18.
The aim of this work is to compare simultaneous isotope dilution analysis of organotin and organomercury compounds by gas chromatography-mass spectrometry (GC-MS) and gas chromatography-inductively coupled plasma mass spectrometry (GC-ICP/MS) on certified bivalve samples. These samples were extracted by microwave with tetramethylammonium hydroxide (TMAH). Derivatization with both NaBEt4 and NaBPr4 was evaluated, and analytical performances were compared. Two CRM materials, BCR-710 and CRM-477, were analyzed by both techniques to verify accuracy. A mixed spike containing (201)Hg-enriched methylmercury (MeHg), (199)Hg-enriched inorganic mercury (iHg), (119)Sn-enriched monobutyltin (MBT), dibutyltin (DBT), and tributyltin (TBT) as well as homemade (116)Sn-enriched monophenyltin (MPT), diphenyltin (DPT), and triphenyltin (TPT) was used for the isotope dilution analysis of samples. The two techniques studied were compared in terms of classic analytical parameters: linearity, precision or repeatability (i.e., percent relative standard deviation, RSD%), limit of detection (LOD), and limit of quantification (LOQ), showing excellent linearity, precision below 12% for all analytes, and LOQs of 0.06-1.45 pg for GC-MS and 0.02-0.27 pg for GC-ICP/MS.
本工作旨在比较用气相色谱-质谱法(GC-MS)和气相色谱-电感耦合等离子体质谱法(GC-ICP/MS)对经认证的双壳贝类样品中有机锡和有机汞化合物进行同位素稀释分析。这些样品用四甲基氢氧化铵(TMAH)经微波提取。评估了与 NaBEt4 和 NaBPr4 的衍生化,并比较了分析性能。用这两种技术分析了两个 CRM 材料,BCR-710 和 CRM-477,以验证准确性。使用混合标准溶液(201)Hg 富集的甲基汞(MeHg)、(199)Hg 富集的无机汞(iHg)、(119)Sn 富集的单丁基锡(MBT)、二丁基锡(DBT)和三丁基锡(TBT)以及自制的(116)Sn 富集的单苯基锡(MPT)、二苯基锡(DPT)和三苯基锡(TPT),对样品进行同位素稀释分析。从经典分析参数方面对两种技术进行了比较:线性、精密度或重复性(即相对标准偏差,RSD%)、检出限(LOD)和定量限(LOQ),结果表明,所有分析物均具有极好的线性,精密度低于 12%,GC-MS 的 LOQs 为 0.06-1.45 pg,GC-ICP/MS 的 LOQs 为 0.02-0.27 pg。