Facultad de Química, Departamento de Química Analítica y Alimentaria, Universidad de Vigo, Vigo, Spain.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2009 Feb;26(2):221-8. doi: 10.1080/02652030802290522.
Conditions for the determination of lipophilic marine toxins, such as yessotoxins and pectenotoxins (PTX)-6, were investigated with capillary electrophoresis coupled to mass spectrometry (MS) with an electrospray ionization source. After optimization, a simple and MS compatible alkaline volatile buffer solution of ammonium acetate was selected as background electrolyte, with isopropanol/water (80/20, v/v) sheath liquid modified with ammonium acetate used at the electrospray ionization (ESI) source. Previously to capillary electrophoresis (CE) separations, the application of an on-line sample pre-concentration approach based on field-amplified sample stacking was accomplished to increase sensitivity. As a result, the limits of detection provided by capillary electrophoresis-electrospray ionization-mass spectrometry (CE-ESI-MS) were 0.02 microg ml(-1) (0.01 microg g(-1)), which corresponded to 1.25 pg for yessotoxin and 0.25 microg ml(-1) (0.13 microg g(-1) and 13.25 pg on capillary) for PTX-6. Accuracy tests showed 97.7% recovery from spiked blank mussel samples that showed no significant matrix influence running under optimal conditions. Intermediate precision was close to 4% relative standard deviation (RSD) for the migration time, and an RSD of 7.5% for peak areas. The method was successfully applied to naturally contaminated seafood samples in which yessotoxins and pectenotoxins-6 were clearly determined. This work demonstrated the potential of CE-ESI-MS to be applied for a sensitive determination of lipophilic toxins from the marine environment as alternative to liquid chromatography-electrospray ionization-single quadrupole mass spectrometry (LC-ESI-MS) for this purpose.
条件下的确定亲脂性海洋毒素,如 yessotoxins 和扇贝毒素 (PTX)-6, 进行了调查与毛细管电泳耦合质谱 (MS) 与电喷雾电离源。经过优化,一个简单和 MS 兼容碱性挥发性缓冲溶液的醋酸铵被选为背景电解质,异丙醇/水 (80/20,v/v) 鞘液改性醋酸铵在电喷雾电离 (ESI) 源。之前毛细管电泳 (CE) 分离,应用在线样品预浓缩方法基于场放大样品堆积来提高灵敏度。作为一个结果,检测限毛细管电泳 - 电喷雾电离质谱 (CE-ESI-MS) 提供了 0.02 microg ml(-1) (0.01 microg g(-1)), 这相当于 1.25 pg yessotoxin 和 0.25 microg ml(-1) (0.13 microg g(-1) 和 13.25 pg 毛细管) 为 PTX-6。准确度测试表明 97.7%回收率从加标空白贻贝样品没有显著基质影响运行在最佳条件下。中间精密度接近 4%相对标准偏差 (RSD) 为迁移时间和 RSD 的 7.5%为峰面积。该方法成功地应用于自然污染海鲜样品中 yessotoxins 和扇贝毒素 - 6 清楚地确定。这项工作表明毛细管电泳的潜力 - ESI-MS 应用于敏感测定亲脂性毒素从海洋环境作为替代液相色谱 - 电喷雾电离 - 单四极杆质谱 (LC-ESI-MS) 为此目的。
