Koyama Masamichi, Yoshida Kazuo, Uchibori Nobutake, Wada Ichirou, Akiyama Kazuyuki, Sasaki Tamami
Laboratory, Japanese Consumers' Co-operative Union, Nishiki-cho, Warabi-shi, Saitama 335-0005, Japan.
Shokuhin Eiseigaku Zasshi. 2005 Jun;46(3):72-8. doi: 10.3358/shokueishi.46.72.
A simple and rapid method for the simultaneous determination of nine kinds of sweeteners (acesulfame potassium, AK; sucralose, SUC; saccharin, SA; cyclamate, CYC; aspartame, APM; dulcin, DU; glycyrrhizic acid, GA; stevioside, STV; rebaudioside A, REB) in various foods by high-performance liquid chromatography-electrospray mass spectrometry (LC/ESI-MS) was developed. The LC separation was performed on a ZORBAX Eclipse XDB-C18 (2.1 mm x 150 mm) with a mobile phase of 5 mmol/L dibutylammonium acetate (DBAA) and acetonitrile-water (8: 2). Mass spectral acquisition was done in the negative ion mode by applying selected ion monitoring (SIM). The sweeteners were extracted from foods with 0.08 mol/L phosphate buffer (pH 7.0)- ethanol (1:1), and the extract was cleaned up on a Sep-pak Vac C18 cartridge after the addition of tetrabutylammonium bromide and phosphate buffer (pH 3.0). The recovery of the nine kinds of sweeteners from five kinds of foods fortified at the level 0.01 g/kg, 0.05 g/kg and 0.20 g/kg was 75.7-109.2%, and the between-day SD values were 0.5-10.9%. The quantification limits of AK, SA, CYC, APM and STV were 0.001 g/kg, and those of SUC, DU, GA and REB were 0.005 g/kg. A recovery test from each cleaned-up sample solution was necessary to detect ionization suppression.
建立了一种利用高效液相色谱 - 电喷雾质谱（LC/ESI-MS）同时测定各类食品中九种甜味剂（乙酰磺胺酸钾，AK；三氯蔗糖，SUC；糖精，SA；甜蜜素，CYC；阿斯巴甜，APM；卫矛醇，DU；甘草酸，GA；甜菊糖苷，STV；莱鲍迪苷A，REB）的简单快速方法。LC分离在ZORBAX Eclipse XDB-C18（2.1 mm×150 mm）色谱柱上进行，流动相为5 mmol/L乙酸二丁铵（DBAA）与乙腈 - 水（8:2）。通过选择离子监测（SIM）在负离子模式下进行质谱采集。甜味剂用0.08 mol/L磷酸盐缓冲液（pH 7.0） - 乙醇（1:1）从食品中提取，提取物在加入溴化四丁铵和磷酸盐缓冲液（pH 3.0）后，在Sep-pak Vac C18柱上进行净化。在0.01 g/kg、0.05 g/kg和0.20 g/kg添加水平下，从五种食品中回收九种甜味剂的回收率为75.7 - 109.2%，日间标准差为0.5 - 10.9%。AK、SA、CYC、APM和STV的定量限为0.001 g/kg，SUC、DU、GA和REB的定量限为0.005 g/kg。为检测电离抑制，需要对每个净化后的样品溶液进行回收率测试。
