HPLC-CAD法同时测定烟用浸膏类香原料中10种水溶性糖  

Simultaneous determination of ten water-soluble sugars in tobacco flavor concretes by HPLC-CAD

作　　者：任家乐 张华[2] 张媛[2] 刘琪[2] 沈海峰 朱怀远[2] 廖惠云[2] 迟波[1] REN Jiale;ZHANG Hua;ZHANG Yuan;LIU Qi;SHEN Haifeng;ZHU Huaiyuan;LIAO Huiyun;CHI Bo(College of Food Science and Light Industry,Nanjing Technology University,Nanjing 211816,China;China Tobacco Jiangsu Industrial Co.,Ltd.,Nanjing 210019,China)

机构地区：[1]南京工业大学食品与轻工学院,南京市211816 [2]江苏中烟工业有限责任公司,南京市210019

出　　处：《烟草科技》2024年第11期1-10,共10页Tobacco Science & Technology

基　　金：中国烟草总公司科技项目“废次烟叶的渗透汽化提取分离耦合技术开发及规模化应用”(110202202024);江苏中烟工业有限责任公司对外合作科技创新项目“复杂基质体系中烟草提取物组分解析及应用研究”(H202228);江苏中烟工业有限责任公司科技创新项目“重点规格功能性香基模块成分剖析及数据库构建”(202108);“高分辨质谱分析常用天然植物提取物及其在仿香中的应用”(202410)。

摘　　要：为了测定烟用浸膏类香原料中水溶性糖的含量,优化并建立了使用高效液相色谱-电喷雾式检测器(HPLC-CAD)的分析方法。通过对色谱分离条件、CAD参数以及样品提取条件等进行系统优化,实现了果糖、阿拉伯糖、鼠李糖、半乳糖、甘露糖、木糖、麦芽糖、葡萄糖、蔗糖和山梨醇10种水溶性糖的有效分离和准确定量。结果表明:①与50%的乙腈水溶液相比,利用水为溶剂的整体萃取效果更好。②色谱条件采用0.4%三乙胺水溶液和乙腈为流动相进行梯度洗脱、流速0.6mg/min和色谱柱温度40℃,且CAD参数为采集频率5Hz、检测室温度50℃和峰宽0.02时,目标物整体上分离效果较佳。③在优化条件下,10种水溶性糖在0.05~1.00mg/mL范围内回归方程相关系数良好(R2均大于0.999),检出限和定量限分别介于0.33~0.60mg/g和1.11~1.99mg/g之间,加标回收率介于80.81%~104.76%之间,日内和日间RSD分别介于1.03%~5.17%和4.42%~6.97%之间。④使用该方法对45个常用烟用浸膏类香原料样品进行普查分析的结果显示,葡萄糖、果糖、麦芽糖、蔗糖和山梨醇5种糖类化合物的检出率较高。该方法结果准确可靠,适用于烟用浸膏类香原料水溶性糖的测定。To determine the water-soluble sugar contents in tobacco flavor concretes,an HPLC-CAD method was established and optimized.Through systematic optimization of chromatographic conditions,CAD parameters,and sample extraction conditions,effective separation and accurate quantification of ten water-soluble sugars,including fructose,arabinose,rhamnose,galactose,mannose,xylose,maltose,glucose,sucrose,and sorbitol,were achieved.The results showed that:1)The overall extraction efficiency was better when water was used as the solvent instead of a 50%aqueous acetonitrile solution.2)The HPLC setup using a gradient elution with a mixture of 0.4%triethylamine in water and acetonitrile,at a flow rate of 0.6 mg/min,while maintaining the column temperature at 40℃,coupled with CAD parameters of a collection frequency of 5 Hz,a detector chamber temperature of 50℃,and a peak width setting of 0.02,provided optimal separation of the target analytes.3)Under the optimized conditions,the linear regression equations for the ten sugars had better correlation coefficients(R2>0.999)in the range of 0.05-1.00 mg/mL,the limits of detection and limits of quantification were in the range of 0.33-0.60 and 1.11-1.99 mg/g,respectively.The recoveries of the analytes ranged from 80.81%to 104.76%,with intraand inter-day RSDs ranging from 1.03%to 5.17%and 4.42%to 6.97%,respectively.4)The method was applied to a survey of 45 commonly used tobacco flavor concrete samples,and the results showed that glucose,fructose,maltose,sucrose,and sorbitol were the five sugar compounds with higher detection rates.The results of this method are accurate and reliable,and it is suitable for the determination of water-soluble sugars in tobacco flavor concretes.

关 键 词：烟用香原料 浸膏 高效液相色谱-电喷雾式检测器 水溶性糖 

分 类 号：TQ656.5[化学工程—精细化工]