高效液相色谱法检测白酒中痕量环己基氨基磺酸钠  

Determination of trace sodium cyclohexyl sulfamate in Baijiu by HPLC

作　　者：魏功 王乐 李春芳 张智洋 任国军 严伟 王慧 WEI Gong;WANG Le;LI Chunfang;ZHANG Zhiyang;REN Guojun;YAN Wei;WANG Hui(Hetao Liquor Industry Group Co.,Ltd.,Bayannur 015400,China)

机构地区：[1]内蒙古河套酒业集团股份有限公司,内蒙古巴彦淖尔015400

出　　处：《中国酿造》2024年第4期247-252,共6页China Brewing

基　　金：内蒙古河套酒业集团股份有限公司项目(HT-2021-JT005)。

摘　　要：该实验建立了一种利用高效液相色谱(HPLC)法检测白酒中痕量环己基氨基磺酸钠(甜蜜素)的方法。根据甜蜜素的热稳定性对白酒样品进行第一次浓缩,衍生后不同萃取溶剂萃取、碱洗后进行二次浓缩,选择不同的溶剂复溶后过膜上机测试,通过流动相试验优化色谱条件,采用单因素试验、正交试验优化前处理条件,再通过方法学考察进行评价。结果表明,最佳前处理条件为称样量100 g、沸水浴浓缩蒸干续蒸0.5 h除去掉白酒中大部分干扰成分、衍生后正庚烷萃取、碱洗后二次浓缩、采用流动相(甲醇∶100 mmol/L乙酸铵水溶液=75∶25,V/V)复溶后液相色谱法测定。该方法在0.01~1 mg/kg范围内标准曲线线性关系良好(R2=0.9998),检出限0.01 mg/kg,定量限0.03 mg/kg,不同香型白酒样品中环己基氨基磺酸钠的加标回收率为94.4%~103.7%,精密度试验结果的相对标准偏差(RSD)为2.70%~3.73%(n=6),该方法准确度较高,精密度良好,适用于各种香型白酒中痕量甜蜜素的检测。A method for the determination of trace sodium cyclamate in Baijiu by HPLC was established.According to the thermal stability of sodium cyclamate,the Baijiu samples were concentrated for the first time,extracted by different solvents after derivatization,and then the samples were concentrated twice after extraction with different extraction solvents and alkali washing.After resolubilization with different solvents,the chromatographic conditions were optimized by mobile phase test,the pretreatment conditions were optimized by single factor tests and orthogonal tests,and then evaluated by methodological investigation.The results showed that the optimal pre-treatment conditions were as follows:weighing sample 100 g,concentrating in boiling water bath,drying and steaming for 0.5 h to remove most of the interfering components in Baijiu,extracting with n-heptane after derivatization,secondary concentrated after alkali washing,and determined by liquid chromatography after mobile phase resolubilization.The results showed that the linear relationship of the standard curve of the method was good in the range of 0.01-1 mg/kg(R2=0.9998),the detection limit was 0.01 mg/kg,and the quantification limit was 0.03 mg/kg.The recovery rate of sodium cyclamate in different flavor Baijiu samples was 94.4%-103.7%,and the relative standard deviation(RSD)of precision test results was 2.70%-3.73%(n=6).The method had high accuracy and good precision,which was suitable for the determination of trace sodium cyclamate in various flavor Baijiu.

关 键 词：环己基氨基磺酸钠 高效液相色谱法 白酒 

分 类 号：TS261.2[轻工技术与工程—发酵工程] R151.3[轻工技术与工程—食品科学与工程]