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Rapid and direct speciation of methyltins in seawater by an on-line coupled high performance liquid chromatography-hydride generation-ICP/MS system

机译:在线耦合高效液相色谱-氢化物发生-ICP / MS系统对海水中的甲基锡进行快速直接形成

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摘要

A novel on-line coupled HPLC-hydride generation (HG)-ICP/MS system was developed for rapid, direct and sensitive speciation of methyltins in seawater without any pretreatment step. Methyltin compounds were separated by reversed phase HPLC, and then on-line reacted with potassium borohydride and acetic acid to generate volatile hydride products. The volatile derivatization products were separated in the spray chamber of ICP/MS and then introduced into ICP/MS by argon gas for detection. Monomethyltin (MMT). dimethyltin (DMT) and trimethyltin (TMT) were baseline separated in less than 15 min by reversed phase HPLC The influence of KBH(4) concentration and type of acid on the system performance was investigated and optimized. Calibration curves, based on peak heights against concentration. were linear in the range of 0.5-50 ng (Sn) mL(-1) of methyltins with correlation coefficients of 0.9990,0.9990 and 0.9996 for MMT, DMT and TMT, respectively. The relative standard deviations measured at 10 ng (Sn) mL-1 for these three methyltins were in the range of 0.6-1.4% (n = 5), and the calculated detection limits (S/N = 3) for MMT, DMT and TMT were 0.266,0.095 and 0.039 ng (Sn) mL(-1), respectively. This method was successfully applied to the speciation of methyltins in seawater with spiked recovery in the range of 95.4-106.9% MMT and DMT were detected in all the seawater samples with concentrations in the range of 1.0-1.5 and 0.30-0.57 ng (Sn) mL(-1) for MMT and DMT, respectively. (C) 2008 Elsevier B.V. All rights reserved.
机译:开发了一种新颖的在线耦合HPLC-氢化物发生(HG)-ICP / MS系统,无需任何预处理步骤即可快速,直接和敏感地鉴定海水中甲基锡的形态。通过反相HPLC分离甲基锡化合物,然后使其与硼氢化钾和乙酸在线反应以生成挥发性氢化物产物。挥发性衍生化产物在ICP / MS喷雾室中分离,然后通过氩气引入ICP / MS进行检测。单甲基锡(MMT)。通过反相HPLC在不到15分钟的时间内将二甲基锡(DMT)和三甲基锡(TMT)进行了基线分离。研究并优化了KBH(4)浓度和酸类型对系统性能的影响。基于峰高对浓度的校准曲线。在0.5-50 ng(Sn)mL(-1)的甲基锡范围内呈线性关系,MMT,DMT和TMT的相关系数分别为0.9990、0.9990和0.9996。这三种甲基锡在10 ng(Sn)mL-1处测得的相对标准偏差在0.6-1.4%(n = 5)的范围内,MMT,DMT和MMT的计算检出限(S / N = 3)。 TMT分别为0.266、0.095和0.039 ng(Sn)mL(-1)。该方法已成功应用于海水中甲基锡的形态分析,加标回收率在95.4-106.9%范围内,在所有海水样品中检出的MMT浓度在1.0-1.5和0.30-0.57 ng(Sn)之间MMT和DMT分别为mL(-1)。 (C)2008 Elsevier B.V.保留所有权利。

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