Chemistry Department, Federal University of São Carlos, SP, Brazil.
Talanta. 2010 Jun 30;82(1):384-91. doi: 10.1016/j.talanta.2010.04.056. Epub 2010 May 21.
This work reports the use of a two-dimensional liquid chromatography (2D-LC) system for quantification of the enantiomers of omeprazole in distinct native aqueous matrices. An octyl restricted-access media bovine serum albumin column (RAM-BSA C(8)) was used in the first dimension, while a polysaccharide-based chiral column was used in the second dimension with either ultraviolet (UV-vis) or ion-trap tandem mass spectrometry (IT-MS/MS) detection. An in-line configuration was employed to assess the exclusion capacity of the RAM-BSA columns to humic substances. The excluded macromolecules had a molecular mass in the order of 18 kDa. Good selectivity, extraction efficiency, accuracy, and precision were achieved employing a very small amount (500 microL or 1.00 mL) of native water sample per injection, with detection limits of 5.00 microg L(-1), using UV-vis, and 0.0250 microg L(-1), using IT-MS/MS. The total analysis time was only 35 min, with no time spent on sample preparation. The methods were successfully applied to analyze a series of waste and estuarine water samples. The enantiomers were detected in an estuarine water sample collected from the Douro River estuary (Portugal) and in an influent sample from the wastewater treatment plant (WWTP) of São Carlos (Brazil). As far as we are concerned, this is the first report of the occurrence of (+)-omeprazole and (-)-omeprazole in native aqueous matrices.
本工作报道了使用二维液相色谱(2D-LC)系统定量分析不同天然水基质中奥美拉唑对映体的方法。在第一维中使用辛基受限-access 介质牛血清白蛋白柱(RAM-BSA C(8)),在第二维中使用多糖基手性柱,并采用紫外(UV-vis)或离子阱串联质谱(IT-MS/MS)检测。采用在线配置评估 RAM-BSA 柱对腐殖质的排除能力。被排除的大分子的分子量约为 18 kDa。采用非常少量(500 μL 或 1.00 mL)天然水样进行进样,采用 UV-vis 检测的检测限为 5.00 μg L(-1),采用 IT-MS/MS 检测的检测限为 0.0250 μg L(-1),可获得良好的选择性、萃取效率、准确度和精密度。总分析时间仅为 35 min,无需花费时间进行样品制备。该方法成功应用于分析一系列废水和河口水样。在从葡萄牙杜罗河口采集的河口水样以及来自巴西圣卡洛斯污水处理厂(WWTP)的进水样中检测到对映体。就我们所知,这是首次在天然水基质中检测到(+)-奥美拉唑和(-)-奥美拉唑的报道。