搅拌棒膜萃取-毛细管电泳分离检测果酱中合成色素胭脂红和苋菜红  

Sensitive Determination of Synthetic Colorants of Carmine and Amaranth in Jam by Membrane Solid Phase Extraction Using Capillary Electrophoresis

作　　者：谭凤玉 王姗姗 谢天尧[1] TAN Fengyu;WANG Shanshan;XIE Tianyao(School of Chemistry,Sun Yat-Sen University,Guangzhou 510275,China)

机构地区：[1]中山大学化学学院,广东广州510275

出　　处：《食品科技》2022年第4期322-328,共7页Food Science and Technology

基　　金：中山大学产学研项目(2018PLR028)。

摘　　要：制备了以搅拌棒为载体的聚己内酰胺膜作为固相萃取剂,对经酸化后的果酱样品溶液中微量胭脂红和苋菜红表现出优异的吸附性能。经过“吸附-脱附”的样品净化处理过程,有效地消除了果酱食品中共存的大量无机盐和有机物基质对于检测微量胭脂红和苋菜红的干扰。结合场放大进样在线富集技术和毛细管电泳非接触式电导法建立了测定果酱中胭脂红和苋菜红的分析方法。对固相萃取过程中实验条件(溶液酸度、萃取时间、洗脱溶剂及洗脱时间等参数)进行了优化,对吸附机制作了初步探讨。以30 mmol/L乙酸+2.0 mmol/L乙酸铵+2.0 mmol/L羟丙基-β-环糊精为电泳运行液,负高压分离(–14 kV),场放大进样(–11 kV×10 s),胭脂红和苋菜红获得良好分离和灵敏检测。检出限为8.1μg/L和8.2μg/L,定量限为25μg/L,实际样品的加标回收率为93.2%~107.3%,相对标准偏差小于7.2%。该法具有灵敏快速、简单高效、分析成本低的优点,可满足市售果酱中合成色素胭脂红和苋菜红的快速灵敏检测要求。A new method was established for sensitive simultaneous determination of carmine and amaranth in jam by capillary electrophoresis(CE)using field-amplified sample injection(FASI)and capacitively coupled contactless conductivity detection(C4D).In order to remove the complex matrix interference co-existing in jam samples,a novel polyamide membrane as a coating adsorbent on the silica stir bar was fabricated.By the membrane solid-phase extraction(mSPE),the complex matrix interferences were effectively removed.Parameters affecting the mSPE efficiency were investigated in detail,including pH value of solution,extraction time,desorption solvent and desorption time.The adsorption mechanism was also discussed briefly.30 mmol/L acetic acid+2.0 mmol/L ammonium acetate+2.0 mmol/L hydroxypropyl-β-Cyclodextrin is the running solution of electrophoresis,with negative high voltage separation(-14 kV)and field amplification injection(-11 kV×10 s),carmine and amaranth obtained good separation and sensitive detection.The limit of detection was 8.1μg/L and 8.2μg/L respectively,and the limit of quantification was 25μg/L.The accuracy was tested by spiking carmine and amaranth standards into jam samples,and the recoveries ranged from 93.2%to 107.3%.The relative standard deviations were below 7.2%.This proposed method can meet the requirements for the fast screening and sensitive detection of carmine and amaranth in jam samples.

关 键 词：膜固相萃取 毛细管电泳 合成色素 胭脂红 苋菜红 果酱 

分 类 号：TS207.5[轻工技术与工程—食品科学]