摘要
建立一种采用超高效液相色谱-串联质谱(UHPLC-MS/MS)法同时测定啤酒中4种嘌呤类生物碱(腺嘌呤、鸟嘌呤、次黄嘌呤、黄嘌呤)的方法。啤酒样品脱气后,经三氟乙酸和甲酸高温水解,采用Agilent Poroshell 120EC-C_(18)(3.0 mm×150 mm,2.7μm)色谱柱进行分离,以甲醇-水作为流动相体系梯度洗脱,在电喷雾电离源(ESI)正离子模式下,以多反应监测模式(MRM)进行定性定量分析。结果表明,4种嘌呤组分在0.5~250μg/L的质量浓度范围内线性关系良好,相关系数(r^(2))均大于0.999,检出限(LOD)为6.0~12μg/L,定量限(LOQ)为20~40μg/L。在腺嘌呤5.04~15.12 mg/L、鸟嘌呤12.76~38.28 mg/L、次黄嘌呤1.32~3.96 mg/L和黄嘌呤2.52~7.56 mg/L加标水平下,平均回收率为80.5%~98.2%,相对标准偏差(δ_(RSD),n=6)为1.3%~4.2%。该方法前处理简单、分析快速、灵敏度高、准确性高,适用于啤酒中4种嘌呤的同时测定。
A method was developed for the determination of four purines(adenine,guanine,hypoxanthine and xanthine)in beer by ultra high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS).The beer sample was degassed and hydrolyzed with trifluoroacetic acid and formic acid,and the chromatographic separation was carried out on an Agilent Poroshell 120 EC-C_(18) column(3.0 mm×150 mm,2.7μm)using methanol-water as mobile phase by gradient elution.The four purines were qualitatively and quantitatively determined by ESI+-MS/MS under multi-reaction monitoring mode(MRM).The results showed that good linear ranges for four purines were obtained from 0.5μg/L to 250μg/L with correlation coefficients(r^(2))larger than 0.999,and the limits of detection(LODs)were within 6.0-12μg/L,while the limits of quantitation(LOQs)were within 20-40μg/L.The mean recoveries of four purines were in the range of 80.5%-98.2%at spiked levels of 5.04-15.12 mg/L for adenine,12.76-38.28 mg/L for guanine,1.32-3.96 mg/L for hypoxanthine and 2.52-7.56 mg/L for xanthine,with relative standard deviations(δ_(RSD),n=6)of 1.3%-4.2%.The optimized method was proved to be simple,rapid,highly sensitive,accurate,and suitable for the determination of four purines in beer.
作者
林钦恒
李圣男
邓远强
郑家概
LIN Qinheng;LI Shengnan;DENG Yuanqiang;ZHENG Jiagai(Guangdong Provincial Engineering Research Center for Efficacy Component Testing and Risk Substance Rapid Screening of Health Food,Guangdong Provincial Key Laboratory of Emergency Test for Dangerous Chemicals,Institute of Analysis,Guangdong Academy of Sciences(China National Analytical Center,Guangzhou),Guangzhou 510070)
出处
《食品工业》
CAS
2021年第6期448-451,共4页
The Food Industry
基金
广东省科学院建设国内一流研究机构行动专项资金项目青年科技工作者引导专项(0105)(项目编号:2019GDASYL-0105014)。
关键词
啤酒
嘌呤
UPLC-MS/MS
测定
beer
purine
ultra performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)
determination