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
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, 1.7 μm)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 of γ－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, 1.7 μm) 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. Results γ－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 of γ-aminobutyric acid.
标题：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
英文标题：Simultaneous determination of γ－aminobutyric acid in pumpkin by ultra performance liquid chromatography-tandem mass spectrometry
作者：
秦宇 上海市质量监督检验技术研究院
侯蓓蓓 上海市质量监督检验技术研究院
张斌骏 上海市质量监督检验技术研究院
葛宇 上海市质量监督检验技术研究院
中文关键词:超高效液相色谱-串联质谱法,γ-氨基丁酸,南瓜,
英文关键词:ultra performance liquid chromatography-tandem mass spectrometry,γ－aminobutyric acid,pumpkin,
发表日期：2019-11-21
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