摘要
建立了高效液相色谱-蒸发光散射检测仪(HPLC-ELSD)同时检测食品中安赛蜜、糖精钠、甜蜜素、三氯蔗糖和阿斯巴甜5种甜味剂的方法。甜味剂经0.1%(v/v)甲酸缓冲液提取后,利用C18固相萃取小柱净化浓缩,以3μmC18柱为分离柱,0.1%(v/v)甲酸(氨水调节pH=3.5)-甲醇(61∶39,v/v)为流动相,经高效液相色谱法分离,蒸发光散射检测器进行检测。结果表明,5种甜味剂在30～1 000 mg/L的范围内,具有良好的线性关系(相关系数大于0.997);在3个添加水平下,样品的平均回收率为85.6%～109.0%,相对标准偏差小于4.0%;方法检出限(LOD,信噪比(S/N)=3)分别为安赛蜜2.5 mg/L、糖精钠3 mg/L、甜蜜素10 mg/L、三氯蔗糖2.5 mg/L及阿斯巴甜5 mg/L。该方法简单、灵敏、操作成本低,可用于不同形态食品中多种甜味剂的同时检测。
A high performance liquid chromatographic method with evaporative light scattering detection （HPLC-ELSD） was developed for the simultaneous determination of five synthetic sweeteners （acesulfame-K, saccharin sodium, sodium cyclamate, sucralose and aspartame） in food. The sweeteners were extracted by 0. 1% （v/v） formic acid buffer solution. The extract of sample was cleaned up and concentrated with solid phase extraction （SPE） cartridge. Thenthe sweeteners were separated on a C 18 column （3 μm） using 0. 1% （v/v） formic acid buffer （ adjusted to pH = 3.5 with aqueous ammonia solution ）-methanol （61 ： 39, v/v） as mobile phase, and finally detected by ELSD. The results showed that the reasonable linearity was achieved for all the analytes over the range of 30 - 1 000 mg/L with the correlation coefficients（r） greater than 0. 997. The recoveries for the five sweeteners ranged from 85.6% to 109.0% at three spiked concentrations with the relative standard deviations （RSDs） lower than 4.0%. The limits of detection （ LODs, S/N= 3 ） were 2.5 mg/L for both acesulfame-K and sucralose, 3 mg/L for saccharin sodium,10 mg/L for sodium cyclamate, and 5 mg/L for aspartame. Themethod is simple, sensitive and low cost, and has been successfully applied to the simultaneous determination of the five synthetic sweeteners in food.
出处
《色谱》
CAS
CSCD
北大核心
2012年第3期292-297,共6页
Chinese Journal of Chromatography
基金
国家自然科学基金项目(21175092
21105064)
国家重大科学仪器设备开发专项(2011YQ150072
2011YQ15007204
2011YQ15007207
2011YQ15007210)
关键词
固相萃取
高效液相色谱
蒸发光散射检测
甜味剂
食品安全
solid-phase extraction （SPE）
high performance liquid chromatography （HPLC）
evaporative light scattering detection （ELSD）
sweeteners
food safety
