al-Rashdan A, Heitkemper D, Caruso J A
Department of Chemistry, University of Cincinnati, Ohio 45221.
J Chromatogr Sci. 1991 Mar;29(3):98-102. doi: 10.1093/chromsci/29.3.98.
Speciation of inorganic lead (Pb2+) and several trialkyllead species (trimethyllead chloride [TML], triethyllead chloride [TEL], and triphenyllead chloride [TPhL]) is investigated using high-performance liquid chromatography (HPLC) with detection by both inductively coupled plasma emission spectroscopy (ICP-AES), and inductively coupled plasma mass spectrometry (ICP-MS). Reversed-phase, ion-pairing, and ion-exchange HPLC modes are studied. Optimal chromatographic conditions for ICP-AES detection include a reversed-phase separation utilizing a step gradient from 10 to 70% methanol. However, the gradient has been found to destabilize the plasma when using ICP-MS detection. An isocratic separation with a 30% methanol mobile phase has been found to be the best compromise between plasma stability and chromatographic resolution. Detection limits using ICP-MS detection are 3 orders of magnitude improved over ICP-AES detection.
使用高效液相色谱法(HPLC),通过电感耦合等离子体发射光谱法(ICP-AES)和电感耦合等离子体质谱法(ICP-MS)检测,对无机铅(Pb2+)和几种三烷基铅物种(氯化三甲基铅 [TML]、氯化三乙基铅 [TEL] 和氯化三苯基铅 [TPhL])进行了形态分析。研究了反相、离子对和离子交换HPLC模式。ICP-AES检测的最佳色谱条件包括使用从10%到70%甲醇的梯度洗脱进行反相分离。然而,已发现使用ICP-MS检测时,该梯度会使等离子体不稳定。已发现使用30%甲醇流动相的等度分离是等离子体稳定性和色谱分辨率之间的最佳折衷方案。与ICP-AES检测相比,使用ICP-MS检测的检测限提高了3个数量级。