摘要
通过优化样品前处理及色谱条件,建立了测定不同剂型保健食品中硫胺素、核黄素、吡哆醇、烟酸、烟酰胺及咖啡因6种组分的高效液相色谱方法。样品经20%甲醇-0.1%磷酸溶液提取,Waters XTERRA RP18色谱柱分离,以癸烷磺酸钠-乙腈离子对体系为流动相,梯度洗脱,二极管阵列检测器检测。硫胺素、核黄素、吡哆醇、烟酸、烟酰胺及咖啡因在一定浓度范围内线性关系良好,相关系数r>0.999,固体样品的方法检出限和定量限分别为15 mg/kg和50 mg/kg,液体样品的方法检出限和定量限分别为1.5 mg/kg和5.0 mg/kg,6个待测物的方法回收率在94.7%~108.5%之间,相对标准偏差为0.1%~4.9%。标准储备液3个月内稳定,6家实验室比对结果一致。本方法可实现保健食品中硫胺素、核黄素、吡哆醇、烟酸、烟酰胺及咖啡因的同时测定。
A high-performance liquid chromatography method for the determination of thiamine,riboflavin,pyridoxine,niacin,niacinamide,and caffeine in different dosage forms of health foods was established by optimizing sample pretreatment and chromatographic conditions.The samples were extracted by 20%methanol-0.1%phosphoric acid solution and separated on Waters XTERRA RP18 column using sodium silane sulfonate-acetonitrile ion pair system as the mobile phase to perform gradient elution.Quantitative analysis was carried out using high performance liquid chromatography with diode array detector.There are good linear relationships for 6 compounds in certain concentration ranges,with correlation coefficients(r)greater than 0.999.The limits of detection(LODs)and limits of quantitation(LOQs)for solid samples were 15 mg/kg and 50 mg/kg,respectively.For liquid samples,the LOD and LOQ were 1.5 mg/kg and 5.0 mg/kg,respectively.The recoveries of the 6 compounds ranged from 94.7%to 108.5%,with relative standard deviations between 0.1%and 4.9%.The standard reserve solution was stable for three months,and method comparison results were consistent among 6 laboratories.This method can achieve simultaneous determination of thiamine,riboflavin,pyridoxine,niacin,niacinamide,and caffeine in healthy foods.
作者
严俊
王兴龙
刘少颖
王小芳
武竹英
任韧
YAN Jun;WANG Xinglong;LIU Shaoying;WANG Xiaofang;WU Zhuying;REN Ren(Hangzhou Center for Disease Control and Prevention(Hangzhou Health Supervision Institution),Hangzhou 310000,China;College of Biotechnology,Tianjin University of Science and Technology,Tianjin 300000,China)
出处
《分析试验室》
北大核心
2025年第9期1357-1364,共8页
Chinese Journal of Analysis Laboratory
基金
推荐性国家标准修订项目(20230859-T-424)资助。
关键词
保健食品
不同剂型
功效成分
同时测定
高效液相色谱法
healthy foods
different dosage forms
functional components
simultaneous determination
high performance liquid chromatography
