HPLC法快速分离和检测食品中微量甜蜜素含量-.docVIP

[作者简介] 王敏(1972-,女,硕士,主管医师,主要从事食品安全与检验研究。 化学测定方法 HPLC法快速分离和检测食品中微量甜蜜素含量 王敏,郭德华,韩丽,邓晓军,杨惠琴,陈墨莲 (上海出入境检验检疫局食品中心,上海 200135 [摘要] 目的:建立快速分离和测定食品中甜蜜素的高效液相色谱技术。方法:甜蜜素在紫外可见光范围内不被吸收,但加入次氯酸钠后,次氯酸钠中的氯将甜蜜素的氨基置换,生成N,N-二氯环己胺,再被正己烷萃取出来,在OD S-C 18 柱上,以乙腈(V:水(V=70:30为流动相进行分离,检测波长314n m,外标法定量。结果:该方法检测低限固体样品为 2m g/kg,液体样品0 5m g/L,回收率71 0%~99 1%。结论:该方法快速简便,灵敏度高,干扰少,适用于大部分食品样品的测定。 [关键词] 高效液相色谱法;食品;甜蜜素(环已基氨基磺酸钠 [中图分类号] O657 7+2 [文献标识码] A [文章编号] 1004-8685(200708-1421-02 An i m proved technique-HPLC for rapid detection of cycla m ate in food W ang M in,Guo D e hua,H an L i,D eng X i ao jun,Yang H ui q i n,Chen M o lian (Shangha i Entry-ex it Inspecti on and Q uaranti ne Bureau,Shanghai200135,China [Abstract] O bjective:T o establish an i m proved techn i que-HPLC f o r t he rap i d detection of sod i u m cycla m a te i n foods M ethod s:T raditi ona lHPLC i s no t suitable f o r the deter m i nation o f cyc l am ate as cycla m a te does no t absorb in the useab l e u ltrav io l et/v isi ble(UV/V ISrange But N,N-dichloridecyc l ohexane can be detected,w hich produced by t he reac ti on be t w een cyc la m ate and hypoch l orous sod i u m a fter add i ng hypoch l orous sod i u m T he a m i dogen o f cyc l am ate w as replaced by t he chlo ri ne N,N-dich l o ridecyc l ohexane w as extrac ted i nto n-hexane fro m t he so l ution and w as separated on OD S-C 18 co l u m n by u si ng a m obil e phase of aceton itr ile(V:w ater(V=70:30at1m l/m i n flo w rate,then detected by ultrav i o let/v i sible(U V/ V ISmon itor at314nm Re s u lts:The detec ti on li m it w as2m g/kg for so li d sa m ples and0 5mg/L for liquid sa m ples T he recov e ries w ere71 0%~99 1% Conc l u tion:Th i s m ethod is s i m p l e,rap i d,sensiti ve and of little interference It can be s uccessfull y applied to the m easure m ent o f cyc l ama te i n food [K ey words] H i gh perfo r mance li qui d chrom atography(HPLC;F ood;Cyc l a m a te 甜蜜素的化学名称为环己基氨基磺酸钠,分子式是C 6H 12 NN aO 3 S,具有水溶性好,甜味清爽,稳定性好,热量低等特性,是一种复合食品添加剂。甜蜜素在我国作为人工甜味剂广