State Key laboratory of Marine Environmental Science, Environmental Science Research Center, Xiamen University, Xiamen, China, 361005.
Rapid Commun Mass Spectrom. 2009 Dec;23(23):3795-802. doi: 10.1002/rcm.4321.
On-line solid-phase extraction (SPE) for pre-concentration and sample cleanup is one strategy to reduce matrix effects and to simultaneously improve detection sensitivity in liquid chromatography/mass spectrometry (LC/MS). This paper describes an on-line SPE-LC/MS method for the determination of tributyltin (TBT) and triphenyltin (TPhT) at trace levels in water samples. The direct coupling of an on-line C18 pre-column to LC/MS was used to pre-concentrate TBT and TPhT at trace levels from waters and to remove interfering matrix effects. Pre-concentration was followed by separation of TBT and TPhT on a C18 column using a mobile phase containing 0.1% (v/v) HCOOH/5 mM HCOONH4 and methanol. While both electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) can be interfaced with MS for the detection of TBT and TPhT, ESI-MS was preferred for this application. The calibration curve for the targets was linear in the concentration range 0.1-30 microg L(-1). The detection limit (signal-to-noise (S/N) ratio = 3) was 0.02 microg L(-1) when 3.0 mL of sample was enriched on the C18 pre-column. The recoveries of TBT and TPhT in spiked waters were from 81.0 to 101.9%. The reproducibilities for the analysis of the standard mixture (10 microg L(-1)) for TBT and TPhT were 13.1 and 5.0%, respectively. The developed method was an easy and fast way to analyze TBT and TPhT in water samples.
在线固相萃取（SPE）是一种用于浓缩和样品净化的策略，可减少基质效应并同时提高液相色谱/质谱（LC/MS）的检测灵敏度。本文描述了一种在线 SPE-LC/MS 方法，用于测定水样中痕量三丁基锡（TBT）和三苯基锡（TPhT）。通过将在线 C18 预柱直接与 LC/MS 耦合，可从水中浓缩痕量的 TBT 和 TPhT，并去除干扰的基质效应。浓缩后，使用含有 0.1%（v/v）甲酸/HCOONH4 和甲醇的流动相在 C18 柱上分离 TBT 和 TPhT。尽管电喷雾电离（ESI）和大气压化学电离（APCI）都可以与 MS 接口用于检测 TBT 和 TPhT，但 ESI-MS 更适合此应用。目标物的校准曲线在 0.1-30 μg/L 的浓度范围内呈线性。当 3.0 mL 样品在 C18 预柱上富集时，检测限（信噪比（S/N）比=3）为 0.02 μg/L。TBT 和 TPhT 在加标水样中的回收率为 81.0-101.9%。TBT 和 TPhT 标准混合物（10 μg/L）分析的重现性分别为 13.1%和 5.0%。所开发的方法是一种快速简便的方法，可用于分析水样中的 TBT 和 TPhT。
