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

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,1.7μm)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50~1000μg/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。

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 0.1l 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.