Reyns Tim, Fraselle Stéphanie, Laza Désiré, Van Loco Joris
Scientific Institute of Public Health, Brussels, Belgium.
Biomed Chromatogr. 2010 Sep;24(9):982-9. doi: 10.1002/bmc.1396.
A sensitive and fast method for the quantification of the illegal dye chrysoidine in aquaculture products with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) is presented. Muscle tissues were made alkaline with sodium hydroxide and extracted with ethyl acetate. After evaporation and subsequent defatting with n-hexane, extracts were directly injected onto the UPLC-column. Chromatography was performed on a C(18) column using 0.1% formic acid in water and an acetonitrile gradient within 6 min. Mass spectrometric analysis was performed in the positive electrospray MS/MS mode. The limit of quantification was 0.25 ng/g, which was 30 times lower than the only previously published method with gas chromatographic detection. A complete validation according to the scientific literature and as defined by the European Union was performed. The applicability of the method was shown in the analysis of more than 50 unknown samples in the framework of a monitoring program.
本文介绍了一种采用超高效液相色谱-串联质谱法（UPLC-MS/MS）定量检测水产养殖产品中非法染料金橙黄的灵敏快速方法。用氢氧化钠将肌肉组织碱化，然后用乙酸乙酯萃取。蒸发后，用正己烷进行后续脱脂处理，提取物直接注入UPLC柱。在C(18)柱上进行色谱分析，流动相为含0.1%甲酸的水溶液和乙腈，在6分钟内进行梯度洗脱。质谱分析采用正电喷雾MS/MS模式。定量限为0.25 ng/g，比之前唯一发表的气相色谱检测方法低30倍。根据科学文献并按照欧盟规定进行了全面验证。在一项监测计划的框架内，对50多个未知样品进行分析，展示了该方法的适用性。
