高效液相色谱法快速测定白酒中8种吡嗪类化合物  

Rapid determination of 8 pyrazine compounds in Baijiu by HPLC

作　　者：龙四红 廖妍俨 孙棣 陈学航 黄家岭 李红洲 梁桂娟 LONG Sihong;LIAO Yanyan;SUN Di;CHEN Xuehang;HUANG Jialing;LI Hongzhou;LIANG Guijuan(Guizhou Institute of Products Quality Inspection&Testing,National Quality Inspection and Supervision Center for Liquor and Manufactured Food,Guiyang 550016,China)

机构地区：[1]贵州省产品质量检验检测院国家酒类及加工食品质量监督检验中心,贵州贵阳550016

出　　处：《中国酿造》2021年第1期176-182,共7页China Brewing

基　　金：国家质检总局科技计划项目(2013QK249)。

摘　　要：建立高效液相色谱-荧光检测器(HPLC-FLD)快速测定白酒中8种吡嗪类化合物含量的方法,并优化样品前处理方法和HPLC色谱条件。结果表明,最佳色谱条件为Phenomenon Gemini 5μC6-Phenyl 110A色谱柱(250 mm×4.6 mm);流动相A为乙腈,B为0.1%磷酸水溶液(pH=2.1),梯度洗脱;流速为1.0 mL/min;激发波长280 nm,发射波长348 nm。标准曲线相关系数R2为0.991~0.998,检出限为0.05~0.24μg/mL,重复性试验结果相对标准偏差(RSD)为1.82%~3.83%,精密度试验结果RSD为1.04%~2.49%,样品加标回收率为86.7%~99.0%。该方法操作简单、快捷,精密度和准确度高,重复性好,能同时将白酒中8种吡嗪类化合物完全分离,可用于白酒中吡嗪类化合物的检测。The method for the rapid determination of the contents of 8 pyrazine compounds in Baijiu(chinese liquor)was determined by high performance liquid chromatography with fluorescence detector(HPLC-FLD),and the pre-treatment method of the sample and HPLC chromatographic conditions were optimized.Results showed that the optimal chromatographic conditions were as follows:Phenomenon Gemini 5μC6-Phenyl 110A column(250 mm×4.6 mm),acetonitrile as mobile phase A and 0.1%aqueous phosphoric acid solution(pH=2.1)as mobile phase B by gradient elution,flow rate 1.0 ml/min.The excitation and emission wavelengths were set as 280 nm and 348 nm,respectively.The correlation coefficient of the standard curve was 0.991-0.998,the detection limit was 0.05-0.24μg/ml,the relative standard deviation(RSD)of the repeatability test results was 1.82%-3.83%,the RSD of the precision test results was 1.04%-2.49%,and the sample recovery rate was 86.7%-99.0%.The method was simple,rapid and could separate 8 kinds of pyrazine compounds in Baijiu,and could be used for the determination of pyrazine compounds in Baijiu.

关 键 词：白酒 高效液相色谱法 吡嗪 

分 类 号：O657.7[理学—分析化学]