超高效液相色谱-串联质谱法测定4种饮料中γ-羟基丁酸及其2种相关物质

Determination of gamma hydroxybutyric acid and its related substances in 4 different beverages by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  γ-羟基丁酸  γ-丁内酯  1,4-丁二醇  饮料

英文关键词:gamma hydroxybutyric acid  gamma butyrolactone  1,4-butanediol  beverages

中文摘要:

      目的 建立超高效液相色谱-串联质谱法测定4种不同饮料基质中γ-羟基丁酸及其相关物质的方法。方法 采用乙腈沉淀蛋白、稀释、过滤、超声等简单的样本前处理方法, 选取Agilent SB-C18 (150 mm×3.0 mm, 1.8 μm) 色谱柱, 流动相为0.02%甲酸水溶液(A)和甲醇(B), 梯度洗脱流速为400 μL/min, 柱温: 40 ℃, 选取电喷雾离子源(electrospray ion source, ESI), 正离子模式下多反应监测模式(multiple reaction monitoring, MRM)进行分析。结果 4种化合物在50~1000 ng/mL的浓度范围内线性关系良好, 相关系数(r2)均不小于0.99, 低中高3个浓度下的平均加标回收率为88.9%~105.7%, 平均相对标准偏差为1.16%~9.83%(n=5)。采用所建立的方法对2批次的问题饮料进行分析, 均准确测定样品中4种化合物的量。结论 该方法样品处理简单, 分析时 间短, 重复性和稳定性良好, 适合做饮料中γ-羟基丁酸及其相关物质的测定。

英文摘要:

      Objective To establish a method for determination of gamma hydroxybutyric acid and its related substances in 4 different matrix beverages by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MSMS). Methods Simple pretreatment methods such as acetonitrile precipitated protein, dilution, filtration and ultrasound were adopted. Agilent SB-C18 (150 mm×3.0 mm, 1.8 μm) column was selected as chromatographic column, the liquid phase was 0.02% formic acid solution (A) and methanol (B), the gradient elution velocity was 400 μL/min, the column temperature was 40 ℃, and electrospray ion source (ESI) and multiple reaction monitoring (MRM) in positive ion mode were selected for analysis. Results Four compounds had good relationships in concentration range of 50-1000 ng/mL, the correlation coefficients (r2) were not less than 0.99, and the average recovery rates were 88.9%-105.7%. Under the 3 different concentrations, the average relative standard deviations were 1.16% to 9.83% (n=5). The established method was used to analyze 2 batches of positive beverage, and the amounts of 4 kinds of compounds in the sample were accurately determined. Conclusion This method is simple, rapid, with good repeatability and good stability, which is suitable for the determination of gamma hydroxybutyric acid and its related substances in beverages.