超高效液相色谱-三重四极杆质谱法测定饮料中的γ-羟基丁酸和γ-丁内酯

Determination of γ-hydroxybutyric acid and γ-butyrolactone in beverages by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  γ-羟基丁酸  γ-丁内酯  超高效液相色谱-三重四极杆质谱法  饮料

英文关键词:γ-hydroxybutyric acid  γ-butyrolactone  ultra performance liquid chromatography-tandem mass spectrometry  beverages

中文摘要:

      目的 建立超高效液相色谱-三重四极杆质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)检测饮料中γ-羟基丁酸(4-hydroxybutanoic acid, GHB)和γ-丁内酯(gamma-butyrolactone, GBL)的含量。方法 样品经稀释后, 采用C18色谱柱(100 mm×2.1 mm, 1.7 μm)进行分离, 用甲醇和0.02%甲酸水作为流动相进行梯度洗脱后上机检测。结果 在50~1000 μg/L内GHB和GBL的浓度与峰面积的线性关系良好, 相关系数均大于0.998。γ-羟基丁酸在饮料中的检出限为0.045 mg/kg, 定量限 为0.15 mg/kg, γ-丁内酯在饮料中的检出限为0.033 mg/kg, 定量限为0.11 mg/kg。该方法在检测4种不同类 型的饮料时, 加标回收率为70%~130%, 相对标准偏差(relative standard deviation, RSD)均小于5.0%(n=6)。 结论 该方法操作简单, 灵敏度高, 准确可靠, 适用于饮料中γ-羟基丁酸和γ-丁内酯的测定。

英文摘要:

      Objective To establish a method for the determination of γ-hydroxybutyric acid (GHB) and γ-butyrolactone (GBL) in beverages by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The sample was separated by C18 (100 mm×2.1 mm, 1.7 μm) column after dilution, and methanol and 0.02% formic acid water were used as mobile phase for gradient elution and then detected by UPLC-MS/MS. Results The concentrations of GHB and GBL had a good linearity with the areas of peak in the range of 50-1000 μg/mL and the correlation coefficients were greater than 0.998. The limit of detection of GHB was 0.045 mg/kg and the limit of quantization was 0.15 mg/kg. The limit of detection of GBL was 0.033 mg/kg and the limit of quantitation was 0.11 mg/kg. The spiked recoveries were 70%-130%, and the relative standard deviations (RSDs) were less than 5.0% (n=6). Conclusion The established method is reliable, accurate and sensitive, which is suitable for detecting GHB and GBL in beverages.