超高效液相色谱-串联质谱法测定南瓜中γ-氨基丁酸的含量

Simultaneous determination of γ-aminobutyric acid in pumpkin by ultra performance liquid chromatography-tandem mass spectrometry

目的建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography/tandem mass spectrometry,UPLC-MS/MS)检测南瓜中γ-氨基丁酸的分析方法。方法南瓜样品用水作为提取剂,在80℃水浴条件提取分离10 min。以Waters ACQUITY UPLC BEH HILIC色谱柱(150 mm×2.1 mm,1.7μm)进行分离,以乙腈和0.1%(V:V)甲酸水溶液为流动相进行梯度洗脱,在电喷雾离子源正离子模式(ESI+)和多反应监测(multiple response monitoring,MRM)模式下进行定性定量分析。结果γ-氨基丁酸在0.10~2.00 mg/L范围内线性关系良好,相关系数(r2)≥0.999,检出限(limit of detection,LOD)为0.10 mg/kg。在低、中、高3个加标水平下的回收率为82.3%~93.8%,相对标准偏差(relative standard deviation,RSD)为1.9%~4.5%。结论该方法灵敏高效,回收率优良,重复性好,适用于γ-氨基丁酸的有效检测。

Objective To establish a method for determination ofγ-aminobutyric acid in pumpkin by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods Pumpkin samples were extracted with water as the extractant,and extracted and separated at 80℃for 10 min.Waters ACQUITY UPLC BEH HILIC column(150 mm×2.1 mm,1.7μm)was used for separation.Gradient elution was performed with acetonitrile and 0.1%(V:V)formic acid as mobile phase qualitative and quantitative analysis was performed in electrospray ion source positive ion mode(ESI+)and multiple reaction monitoring(MRM)mode.Resultsγ-aminobutyric acid had good linear relationship in the range of 0.10 to 2.00 mg/L with the correlation coefficients(r2)higher than 0.999.The limit of detection(LOD)was 0.10 mg/kg.The recovery rate at the 3 levels of low,medium and high was 82.3%-93.8%.The relative standard deviation(RSD)was 1.9%-4.5%(n=6).Conclusion This method is sensitive and efficient,and has excellent recovery and good repeatability,which is suitable for the effective detection ofγ-aminobutyric acid.