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建立了液相色谱-串联质谱法测定水产加工品中甜蜜素的测定方法。样品用水提取,正己烷净化后,以0.1%甲酸-甲醇为流动相,C18色谱柱分离,在负离子模式下用配有电喷雾离子源的液相色谱-串联质谱测定。甜蜜素含量1~200 ng/m L范围内,线性关系良好(r~2=0.9999);方法定量限5μg/kg(S/N≥10)。甜蜜素在5μg/kg和50μg/kg添加水平下,平均回收率为81.0%~88.4%,相对标准偏差为4.0%~6.4%。方法适合水产加工品中甜蜜素的测定。本文根据甜蜜素的性质,选取水为提取剂,并对净化方法进行了研究,通过正已烷液-液萃取和冷冻方式去除了提取液中的油类物质和水溶性蛋白,确保了分析结果的稳定性和准确性。该技术的建立为水产加工品中甜蜜素监管提供技术支撑。
A method for the determination of sodium cyclamate in aquatic products by liquid chromatography-tandem mass spectrometry was established. The sample was extracted with water and purified with n-hexane. The sample was separated on a C18 column using 0.1% formic acid-methanol as the mobile phase and analyzed by liquid chromatography-tandem mass spectrometry with an electrospray ionization source in negative ion mode. There was a good linearity (r ~ 2 = 0.9999) for cyclamate content in the range of 1 ~ 200 ng / m L; the limit of quantification was 5 μg / kg (S / N≥10). The average recoveries of cyclamate at 5μg / kg and 50μg / kg were 81.0% ~ 88.4% with relative standard deviations of 4.0% ~ 6.4%. The method is suitable for the determination of cyclamate in aquatic products. In this paper, according to the nature of sodium cyclamate, water was selected as the extractant, and purification methods were studied by n-hexane liquid-liquid extraction and freezing method to remove the oil and water-soluble protein extract to ensure that the analysis results The stability and accuracy. The establishment of this technology provides technical support for the regulation of sodium cyclamate in aquatic products.