| 摘要: |
| 基于稳定同位素内标（SIIS）,构建了一种简单的乳制品前处理方法,将乳制品中的L-岩藻糖（L-Fuc）高效地游离出来,利用高效液相色谱串联质谱法（LC-MS/MS）建立了乳制品中L-岩藻糖含量的定量测定方法. 首次引入SIIS来定量乳制品中的L-岩藻糖,采用电喷雾离子源（ESI）负离子扫描模式和多重反应监测（MRM）模式进行定量分析. 研究过程中对质谱鉴定、色谱条件、样品前处理过程都进行了方法的比较优化,并检测了纯牛奶、酸奶等5种乳制品中L-岩藻糖的含量. L-岩藻糖在0.001~1.000 μg·mL-1范围内线性关系良好,相关系数为0.999 99,样品加标回收率在71.67%~117.27%之间,相对标准偏差（RSD）在2.00%~9.64%之间,检出限为0.1 ng·mL-1,定量限为0.5 ng·mL-1. 该方法样品前处理简单,灵敏度高,检测结果准确,可定量不同乳制品中L-岩藻糖的含量,为其他领域中L-岩藻糖含量的测定提供了可借鉴的方法. |
| 关键词: L-岩藻糖（L-Fuc） 稳定同位素内标（SIIS） 液相色谱串联质谱法（LC-MS/MS） 多重反应监测（MRM） 乳制品 |
| DOI：10.3969/J.ISSN.1000-5137.2024.01.005 |
| 分类号:O 65 |
| 基金项目:上海市科技创新行动计划（20JC1416800） |
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| Determination of L-fucose content in dairy products by high performance liquid chromatography-tandem mass spectrometry with stable isotope internal standard |
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YANG Qianqian, HE Shu, CAO Jing
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College of Chemistry and Materials Science, Shanghai Normal University, Shanghai 200234, China
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| Abstract: |
| Based on the stable isotope internal standard（SIIS）, a simple dairy pretreatment method was established to efficiently separate the L-fucose（L-Fuc） from dairy products. A quantitative method for L-fucose content in dairy products was established using high performance liquid chromatography-tandem mass spectrometry（LC-MS/MS）. SIIS coupled with LC-MS/MS to quantify L-fucose was employed for the first time. The method used electronic spray ionization（ESI） mode and multi reaction monitoring（MRM） mode for quantitative analysis. During the study, the mass spectrometric identification, chromatographic conditions, and sample preparation were optimized, and the content of L-fucose in five kinds of dairy products, such as pure milk and yogurt, was detected. The results showed that the linear range of L-fucose was 0.001-1.000 μg·mL-1, and the correlation coefficient was 0.999 99. The recoveries were 71.67%-117.27%, and the relative standard deviations（RSD） were 2.00%-9.64%. The limit of detection was 0.1 ng·mL-1, and the limit of quantification was 0.5 ng·mL-1. This method has the advantages of simple sample preparation, high sensitivity, accurate detection results, and can be used to quantify the L-fucose in different dairy products. It provides a reference method for the determination of L-fucose content in other fields. |
| Key words: L-fucose（L-Fuc） stable isotope internal standard（SIIS） liquid chromatography-tandem mass spectrometry（LC-MS/MS） multi reaction monitoring（MRM） dairy products |
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