Levine Keith E, Young Daniel J, Afton Scott E, Harrington James M, Essader Amal S, Weber Frank X, Fernando Reshan A, Thayer Kristina, Hatch Elizabeth E, Robinson Veronica G, Waidyanatha Suramya
RTI International, Research Triangle Park, NC, United States.
Division of National Toxicology Program, NIEHS, Research Triangle Park, NC, United States.
Talanta. 2015 Aug 1;140:115-121. doi: 10.1016/j.talanta.2015.03.022. Epub 2015 Mar 27.
Organotin compounds (OTCs) are heavily employed by industry for a wide variety of applications, including the production of plastics and as biocides. Reports of environmental prevalence, differential toxicity between OTCs, and poorly characterized human exposure have fueled the demand for sensitive, selective speciation methods. The objective of this investigation was to develop and validate a rapid, sensitive, and selective analytical method for the simultaneous determination of a suite of organotin compounds, including butyl (mono-, di-, and tri-substituted) and phenyl (mono-, di-, and tri-substituted) species in human serum. The analytical method utilized ultra-performance liquid chromatography (UPLC) coupled with sector field inductively coupled plasma mass spectrometry (SF-ICP-MS). The small (sub-2 µm) particle size of the UPLC column stationary phase and the sensitivity of the SF-ICP-MS enabled separation and sensitive determination of the analyte suite with a runtime of approximately 3 min. Validation activities included demonstration of method linearity over the concentration range of approximately 0.250-13.661 ng mL(-1), depending on the species; intraday precision of less than 21%, interday precision of less than 18%, intraday accuracy of -5.3% to 19%, and interday accuracy of -14% to 15% for all species; specificity, and matrix impact. In addition, sensitivity, and analyte stability under different storage scenarios were evaluated. Analyte stability was found to be limited for most species in freezer, refrigerator, and freeze-thaw conditions. The validated method was then applied for the determination of the OTCs in human serum samples from women participating in the Snart-Foraeldre/MiljØ (Soon-Parents/Environment) Study. The concentration of each OTC ranged from below the experimental limit of quantitation to 10.929 ng tin (Sn) mL(-1) serum. Speciation values were confirmed by a total Sn analysis.
有机锡化合物(OTCs)在工业上被大量用于各种应用,包括塑料生产和用作杀生剂。关于环境中OTCs的普遍存在、不同OTCs之间的毒性差异以及人类暴露情况特征不明的报道,推动了对灵敏、选择性的形态分析方法的需求。本研究的目的是开发并验证一种快速、灵敏且选择性的分析方法,用于同时测定人血清中的一组有机锡化合物,包括丁基(单取代、二取代和三取代)和苯基(单取代、二取代和三取代)化合物。该分析方法采用超高效液相色谱(UPLC)与扇形场电感耦合等离子体质谱(SF-ICP-MS)联用。UPLC柱固定相的小粒径(小于2 µm)以及SF-ICP-MS的灵敏度使得能够在约3分钟的运行时间内分离并灵敏测定分析物组。验证活动包括证明方法在约0.250 - 13.661 ng mL⁻¹的浓度范围内呈线性,具体取决于化合物种类;所有化合物的日内精密度小于21%,日间精密度小于18%,日内准确度为 -5.3%至19%,日间准确度为 -14%至15%;特异性以及基质影响。此外,还评估了不同储存条件下的灵敏度和分析物稳定性。结果发现,在冷冻、冷藏和冻融条件下,大多数化合物的分析物稳定性有限。然后将经过验证的方法应用于参加Snart-Foraeldre/MiljØ(Soon-Parents/Environment)研究的女性的人血清样本中OTCs的测定。每种OTCs的浓度范围从低于实验定量限到10.929 ng锡(Sn)mL⁻¹血清。通过总锡分析确认了形态分析值。