Lab of Analytical Chemistry, Department of Chemistry, Aristotle University, Thessaloniki, Greece.
J Sep Sci. 2010 Jun;33(11):1610-6. doi: 10.1002/jssc.200900661.
A headspace solid-phase microextraction (HS-SPME) method coupled to GC-MS was developed in order to determine trace levels of tetramethyltin (TeMT) and inorganic tin (iSn) after ethylation to tetraethyltin (TeET) in various matrices. The derivatization of iSn and the extraction of both TeMT and iSn as TeET were performed in one step. Sodium tetraethylborate (NaBEt(4)) was used as derivatization agent and the volatile derivatives were absorbed on a PDMS-coated fused silica fiber. The conditions for the HS-SPME procedure were optimized in order to gain in repeatability and sensitivity. Several critical parameters of GC-MS were also studied. The detection of TeMT and iSn as TeET peaks was performed by the SIM mode. The precision of the proposed method is satisfactory providing RSD values below 10% for both tin species and good linearity up to 10 microg/L. The developed method was successfully applied to the determination of tin species in several samples like canned fish, fish tissues, aquatic plants, canned mineral water and sea water. The proposed HS-SPME-GC-MS method was proved suitable to monitor the concentration levels of toxic tin compounds in environmental and biological samples.
建立了顶空固相微萃取（HS-SPME）与 GC-MS 联用方法，用于测定各种基质中经乙基化生成四乙基锡（TeET）后痕量的四甲基锡（TeMT）和无机锡（iSn）。iSn 的衍生化和 TeMT 和 iSn 作为 TeET 的萃取在一步中进行。四乙基硼酸钠（NaBEt（4））用作衍生化试剂，挥发性衍生物被吸收到涂有 PDMS 的熔融石英纤维上。优化了 HS-SPME 程序的条件，以提高重复性和灵敏度。还研究了 GC-MS 的几个关键参数。通过选择离子监测（SIM）模式检测 TeMT 和 iSn 作为 TeET 峰。该方法的精密度令人满意，两种锡形态的 RSD 值均低于 10%，线性良好，可达 10μg/L。该方法成功应用于罐装鱼、鱼组织、水生植物、罐装矿泉水和海水等几种样品中锡形态的测定。所提出的 HS-SPME-GC-MS 方法适用于监测环境和生物样品中有毒锡化合物的浓度水平。
