腐殖酸键合硅胶固相萃取-液相色谱法测定辣椒粉及辣椒油中的苏丹红  

Determination of Sudan Red Dyes in Hot Chili Products by Humic Acid-Bonded Silica Solid-Phase Extraction Coupled with High Performance Liquid Chromatography

作　　者：郑明明[1] 吴剑虹[1] 骆丹[1] 余琼卫[1] 冯钰锜[1] 

机构地区：[1]武汉大学化学与分子科学学院,湖北武汉430072

出　　处：《色谱》2007年第5期619-622,共4页Chinese Journal of Chromatography

基　　金：教育部"新世纪优秀人才支持计划"基金(NCET-05-0616);国家杰出青年科学基金(No20625516)资助项目

摘　　要：以腐殖酸键合硅胶作为固相萃取介质,建立了固相萃取柱净化、高效液相色谱同时检测辣椒粉及辣椒油中苏丹红Ⅰ,Ⅱ,Ⅲ和Ⅳ的方法。该萃取材料对4种苏丹红表现出较强的萃取能力。样品采用正己烷提取,提取液经固相萃取柱净化,通过清洗除去样品中的天然色素和油脂干扰,再用乙醇-二氯甲烷(体积比为3:7)解吸。上述4种苏丹红组分在其质量浓度为0.05～5mg/L的范围内具有良好的线性关系,相关系数的平方均大于0.999;方法的检出限分别为19.8～28.8ng/g(辣椒粉)和7.9～11.5ng/g(辣椒油);日内及日间相对标准偏差分别小于9.1%和8.8%。在实际样品检测中,4种苏丹红的回收率为82.6%～94.0%。结果表明,该方法能较好地去除基质干扰,具有简单、快速、灵敏的特点,适用于食品中苏丹红的常规分析。Humic acid-bonded silica was prepared and used as solid-phase extraction material for the pretreatment of Sudan Red dyes in hot chili products, which was followed by high performance liquid chromatographic determination. This sorbent exhibits an excellent adsorption capacity for Sudan Red dyes. A sample was first extracted with n-hexane. Then the extract was cleaned up by humic acid-bonded silica cartridge and eluted with ethanol/dichloromethane （3： 7, v/v）. Some interferences in hot chili products such as natural pigments and oil were removed by washing step. Good linearities were achieved in the range from 0.05 to 5 mg/L for four Sudan dyes, with linear coefficient r2 values above 0. 999. The limits of detection （LOD） in chili powder and chili oil were from 19.8 to 28.8 ng/g and 7.9 to 11.5 ng/g, respectively. Excellent method reproducibility was found by intra- and inter-day precisions （the relative standard deviations less than 9.1% and 8.8%, respectively）. Recoveries for them in the real samples were between 82.6% and 94.0%. The proposed method is proved to be simple, rapid, and sensitive in the regular analysis of Sudan Red Ⅰ , Ⅱ ,Ⅲ and Ⅳ in foods

关 键 词：腐殖酸 固相萃取 高效液相色谱 苏丹红 

分 类 号：O658[理学—分析化学]