酒类产品中γ-氨基丁酸的测定及其膳食风险评估

Determination ofγ-aminobutyric acid in wines and its dietary risk assessment

建立酒类产品中γ-氨基丁酸含量的测定方法,测定了实际样品并评估了酒类中γ-氨基丁酸的膳食风险水平。通过对提取溶剂、提取方式、色谱及质谱条件进行优化,确立样品采用水直接超声提取,经Agilent Zorbax HILIC(2.1 mm×100 mm,3.5μm)色谱柱分离,以5 mmol/L乙酸铵-乙腈进行梯度洗脱,经高效液相色谱-串联质谱进行定性和定量分析。结果表明,γ-氨基丁酸在1~200μg/L内具有良好的线性关系,R≥0.999;方法检出限和定量限分别为5、10μg/kg;在10、20、100μg/kg加标水平下的回收率为96%~98%(n=6),相对标准偏差<10%,该方法前处理简便快速、灵敏度和选择性强,适用于酒类产品中γ-氨基丁酸的测定。实际样品测定结果表明γ氨基丁酸在242批酒产品中的含量为ND~73 mg/L,4种酒中γ-氨基丁酸的膳食危害熵值为0.0000385,远低于临界值1,消费者食用安全性较高。

A detection method is established for the detection ofγ-aminobutyric acid and the content ofγ-aminobutyric acid was measured and its dietary risk level was evaluated in wines.The extraction solvent and method,chromatography and mass spectrometry conditions were optimized.Samples were extracted with water under ultrasound conditions.The 5mmol/L ammonium acetate-acetonitrile was used for gradient elution and the Agilent Zorbax HILIC column was used for separation.Target compounds were qualitatively and quantitatively analyzed in the ESI+mode and MRM mode.It showed that theγ-aminobutyric acid had a good linear relationship in the range of 1-200μg/L,R≥0.999.The detection limit and the quantification limit range were 5μg/kg and 10μg/kg,respectively.The recoveries of the three spiked levels of 10,20,100μg/kg were 96%-105%(n=6),with a relative standard deviation of<10%.This method applies to the determination ofγ-aminobutyric acid in wines with the advantages of simple and fast pre-treatment,strong sensitivity and selectivity.Results showed that the content ofγ-aminobutyric acid was ND-73.0 mg/L in 242 batches of wines and the dietary hazard quotient(HI)ofγ-aminobutyric acid in the four types of alcohol was 0.0000385,which was far below the critical value of 1,indicating that consumers had a high level of food safety.