高效液相色谱-分段检测法同时测定烟草中14种多酚类化合物  

Simultaneous Determination of Fourteen Polyphenols in Tobacco by Piecewise Detection Based on Liquid Chromatography

作　　者：欧阳璐斯[1] 赖燕华[1] 王予[1] 陶红[1] 黄翼飞[1] OUYANG Lu-si;LAI Yan-hua;WANG Yu;TAO Hong;HUANG Yi-fei(Technology Centre,China Tobacco Guangdong Industrial Co.Ltd.,Guangzhou 510385,China)

机构地区：[1]广东中烟工业有限责任公司技术中心,广东广州510385

出　　处：《分析测试学报》2021年第3期411-416,共6页Journal of Instrumental Analysis

基　　金：广东中烟工业有限责任公司资助项目(粤烟工[2017]科字第9号)。

摘　　要：利用高效液相色谱-二极管阵列检测器(HPLC-DAD),建立了同时分析烟草中新绿原酸、绿原酸、隐绿原酸、东莨菪苷、咖啡酸、七叶亭、对香豆酸、阿魏酸、莨菪亭、7-羟基香豆素、芦丁、槲皮苷、山奈酚-3-O-芸香糖苷和槲皮素14种多酚化合物的方法。称取0.02 g烟末,加入5 mL 50%甲醇,超声萃取30 min,取上清液过水相滤膜后,采用Agilent SB-C18柱(3.0 mm×150 mm,1.8μm)进行分离,以0.05 mol/L磷酸二氢钾水溶液和甲醇为流动相,采用分段式检测,获得14种多酚类化合物在各自最佳检测波长下的信号,实现了良好分离。结果表明,14种多酚类化合物的色谱峰面积与其质量浓度呈良好的线性关系,相关系数r2>0.9997,检出限为0.01~0.15μg/mL,定量下限为0.03~0.50μg/mL,日内相对标准偏差(RSD)为0.70%~3.6%,日间RSD为4.0%~6.4%,加标回收率为95.2%~109%。该方法具有良好的灵敏度、精密度和回收率,适合于烟草样品中多种多酚类化合物的同时测定。A high performance liquid chromatography with diode array detector(HPLC-DAD)was developed for the simultaneous determination of 14 polyphenols,including neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,scopolin,caffeic acid,esculetin,p-coumaric acid,ferruric acid,scopoletin,7-hydroxycoumarin,rutin,quercitrin,kaempferol 3-O-β-rutinoside and quercetin.0.02 g tobacco powder sample was ultrasonically extracted with 5 mL of 50%methanol for 30 min,and then the supernatant was put to pass through an aqueous phase filtration membrane.14 polyphenols were separated at their optimal detection wavelengths on an Agilent SB-C18 column(3.0 mm×150 mm,1.8μm),with 0.05 mol/L potassium dihydrogen phosphate aqueous solution and methanol as mobile phases.There existed good linear relationships between peak areas and mass concentrations of the analytes,with their correlation coefficients(r2)larger than 0.9997.The limits of detection and limits of quantitation were in the ranges of 0.01-0.15μg/mL and 0.03-0.50μg/mL,while the intra-day and inter-day relative standard deviations(RSD)were 0.70%-3.6%and 4.0%-6.4%,respectively.The spiked recoveries ranged from 95.2%to 109%.The proposed method could be applied to the simultaneous determination of a variety of polyphenols in tobacco and cigarettes with good sensitivity,precision and recovery.

关 键 词：高效液相色谱 二极管阵列检测器 分段检测 烟草 多酚 

分 类 号：O657.7[理学—分析化学] TS41[理学—化学]