Nash Martin J, Maskall John E, Hill Steve J
School of Earth, Ocean & Environmental Sciences, University of Plymouth, Drake Circus, Plymouth PL4 8AA, UK.
Analyst. 2006 Jun;131(6):724-30. doi: 10.1039/b600155f. Epub 2006 May 8.
Novel HPLC-ICP-MS methodologies are developed using strong anion exchange (Phenomenex SAX-SB) and weak anion exchange (Alltec HAAX) stationary phases in conjunction with a range of aqueous mobile phases to enable simultaneous separations of inorganic Sb(III), Sb(V) and organic trimethylantimony dichloride (TMSb) species in synthetic solutions. Optimum isocratic separations of inorganic Sb(V) and Sb(III) species are achieved using mobile phases comprised of ammonium tartrate under controlled pH conditions, and rapid pH gradient elution profiles are developed to facilitate separations of the Sb(V), Sb(III) and TMSb species in a single chromatographic run. Optimum peak resolution is achieved when using the 100 x 4.6 mm HAAX column at 20 degrees C and 100 mM ammonium tartrate mobile phases with a gradient from pH 3.0 to pH 1.2, although a system peak co-elutes with TMSb under these conditions and precludes quantitative analyses. Interestingly, the elution order of Sb(V), Sb(III) and TMSb species reverses when the temperature of the HAAX stationary phase is increased to 60 degrees C, and concurrent use of a less acidic pH gradient elution profile from pH 2.3 to pH 1.5 is shown to enable successful species separations whilst preventing occurrence of the co-eluting system peak. Limits of detection are achieved in the sub ng mL(-1) range using these novel HPLC-ICP-MS methodologies and provide scope for future environmental analysis applications.
开发了新型高效液相色谱 - 电感耦合等离子体质谱联用（HPLC - ICP - MS）方法，该方法使用强阴离子交换（菲罗门SAX - SB）和弱阴离子交换（Alltec HAAX）固定相，并结合一系列水性流动相，以实现合成溶液中无机三价锑（Sb(III)）、五价锑（Sb(V)）和有机二氯三甲基锑（TMSb）物种的同时分离。在受控的pH条件下，使用由酒石酸铵组成的流动相可实现无机Sb(V)和Sb(III)物种的最佳等度分离，并开发了快速pH梯度洗脱曲线，以便在一次色谱运行中促进Sb(V)、Sb(III)和TMSb物种的分离。在20℃下使用100×4.6 mm HAAX柱和100 mM酒石酸铵流动相，pH从3.0梯度至1.2时可实现最佳峰分辨率，不过在此条件下有一个系统峰与TMSb共洗脱，妨碍了定量分析。有趣的是，当HAAX固定相温度升至60℃时，Sb(V)、Sb(III)和TMSb物种的洗脱顺序会颠倒，同时使用从pH 2.3至pH 1.5的酸性较低的pH梯度洗脱曲线，可成功实现物种分离，同时防止共洗脱系统峰的出现。使用这些新型HPLC - ICP - MS方法可实现亚纳克每毫升（ng mL⁻¹）范围内的检测限，为未来的环境分析应用提供了空间。
Zotero 插件