离子交换固相萃取-反相高效液相色谱法测定黄酒中游离嘌呤

Determination of free purines in Huangjiu by ion-exchange solid phase extractioncombined with reverse phase high performance liquid chromatography

建立了离子交换固相萃取-反相高效液相色谱法同时测定黄酒中游离鸟嘌呤、次黄嘌呤、黄嘌呤和腺嘌呤的分析方法,并对15批次酒样中4种游离嘌呤进行了测定。样品煮沸除去乙醇后,经MCX混合阳离子交换固相萃取柱净化后,可用高效液相色谱进行分析检测。结果表明,在0.1~25 mg/L质量浓度范围内,鸟嘌呤、次黄嘌呤、黄嘌呤和腺嘌呤的标准曲线线性良好(R>0.9999),4种嘌呤检出限分别为0.1、0.1、0.2、0.1 mg/L,回收率为83.13%~98.32%,4种分析物的日内和日间测定精密度均小于4.0%。此方法简便,快捷,可靠。

A high performance liquid chromatographic method was developed for the simultaneous determination of free guanine,hypoxanthine,xanthine and adenine in 15 Huangjiu(Chinese rice wine)samples.To reduce matrix interferences and increase method sensitivity,MCX mixed cation exchange solid phase extraction column was employed for sample clean-up.After the sample was boiled to remove ethanol,it was purified by MCX column and analyzed by high performance liquid chromatography.The standard curve of purines showed good linearity in the range of 0.1-25 mg/L,with the correlation coefficient R larger than 0.9999.The lowest detectable concentrations of guanine,hypoxanthine,xanthine and adenine were 0.1,0.1,0.2,0.1 mg/L,respectively.The recovery rates were between 83.13%-98.32%.The intra-day and inter-day assay precision(RSD)of these four purines were less than 4.0%.This method is simple,fast and reliable.