Wuilloud Rodolfo G, Shah Monika, Kannamkumarath Sasi S, Altamirano Jorgelina C
University of Cincinnati [corrected] Cincinnati, OH 45221-0172, USA.
Electrophoresis. 2005 Apr;26(7-8):1598-605. doi: 10.1002/elps.200410098.
In this work, the potential of inductively coupled plasma-mass spectrometry (ICP-MS) coupled to capillary electrophoresis (CE) to determine organophosphorus pesticides (OPPs) is demonstrated. Element specific detection of (31)P with ICP-MS is performed for the detection of OPPs. Three common OPPs, including glyphosate, glufosinate, and aminomethylphosphonic acid (AMPA), were analyzed by CE-ICP-MS to demonstrate its applicability for the analysis of OPPs. The advantages of using ICP-MS with respect to other common detectors, such as flame photometric detection (FPD), for CE analysis of OPPs are shown. Additionally, different CE separation conditions were studied to achieve complete baseline separation of the pesticide compounds in short migration times. Two CE buffer systems were evaluated for the separation of OPPs using ICP-MS detection. A buffer solution containing 40 mmol.L(-1) ammonium acetate at pH 9.0 and an applied voltage of +20 kV were finally selected leading to a separation time of 10.0 min. Both migration time and area relative standard deviations (%RSD) were evaluated and their respective values were in the intervals of 1.1-3.3% and 2.7-5.3%. Detection limits obtained with the CE-ICP-MS system were in the range of 0.11-0.19 mg.L(-1) (as compound) yielding an enhancement of 130- to 230-fold with respect to FPD. The proposed methodology was finally applied for the determination of the OPPs mentioned above in natural river water samples.
在本研究中，展示了电感耦合等离子体质谱法（ICP-MS）与毛细管电泳（CE）联用测定有机磷农药（OPPs）的潜力。采用ICP-MS对（31）P进行元素特异性检测以测定OPPs。通过CE-ICP-MS分析了三种常见的OPPs，包括草甘膦、草铵膦和氨甲基膦酸（AMPA），以证明其在OPPs分析中的适用性。展示了在OPPs的CE分析中，使用ICP-MS相对于其他常用检测器（如火焰光度检测（FPD））的优势。此外，研究了不同的CE分离条件，以在短迁移时间内实现农药化合物的完全基线分离。评估了两种CE缓冲体系用于使用ICP-MS检测分离OPPs。最终选择了pH 9.0的含40 mmol·L⁻¹乙酸铵的缓冲溶液和 +20 kV的施加电压，分离时间为10.0分钟。评估了迁移时间和面积相对标准偏差（%RSD），其各自的值在1.1 - 3.3%和2.7 - 5.3%的区间内。CE-ICP-MS系统获得的检测限在0.11 - 0.19 mg·L⁻¹（以化合物计）范围内，相对于FPD提高了130至230倍。最终将所提出的方法应用于天然河水样品中上述OPPs的测定。
