Ji Chao, Feng Feng, Chen Zhengxing, Sun Li, Chu Xiaogang
State Key Laboratory of Food Science and Technology, Jiangnan University, Wuxi 214036, China.
Se Pu. 2010 Aug;28(8):749-53. doi: 10.3724/sp.j.1123.2010.00749.
A high performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI MS/MS) method for the determination of five synthetic sweeteners (acesulfame, sodium saccharin, sodium cyclamate, aspartame and neotame) in wines has been developed. The HPLC separation was carried out on an Ultimate C18 column (100 mm x 2.1 mm, 3 microm). Several parameters, including the composition and pH of the mobile phase, column temperature and the monitor ions, were optimized for improving the chromatographic performance and the sensitivity of determination. The results demonstrated that the separation can be completed in less than 5 min by gradient elution with 20 mmol/L ammonium formate and 0.1% (v/v) formic acid (pH 3.8) and methanol as the mobile phase. The column temperature was kept at 45 degrees C. When the analytes were detected by ESI -MS/MS under multiple reaction monitoring mode, the detection limits were 0.6, 5, 1, 0.8 and 0.2 microg/L for acesulfame, sodium saccharin, sodium cyclamate, aspartame and neotame, respectively. The average recoveries ranged from 87.2% to 103%. The relative standard deviations were not more than 1.2%. This method is rapid, accurate, highly sensitive and suitable for the quality control of low concentration of the synthetic sweeteners, which are illegally added to wines and other foods with complex matrices.
建立了一种用于测定葡萄酒中五种合成甜味剂(乙酰磺胺酸钾、糖精钠、环己基氨基磺酸钠、阿斯巴甜和纽甜)的高效液相色谱 - 电喷雾电离串联质谱(HPLC - ESI MS/MS)方法。HPLC分离在Ultimate C18柱(100 mm×2.1 mm,3μm)上进行。对包括流动相组成和pH、柱温以及监测离子在内的几个参数进行了优化,以提高色谱性能和测定灵敏度。结果表明,以20 mmol/L甲酸铵和0.1%(v/v)甲酸(pH 3.8)与甲醇作为流动相进行梯度洗脱,可在不到5分钟内完成分离。柱温保持在45℃。当在多反应监测模式下通过ESI - MS/MS检测分析物时,乙酰磺胺酸钾、糖精钠、环己基氨基磺酸钠、阿斯巴甜和纽甜的检测限分别为0.6、5、1、0.8和0.2μg/L。平均回收率在87.2%至103%之间。相对标准偏差不超过1.2%。该方法快速、准确、高度灵敏,适用于对非法添加到葡萄酒和其他复杂基质食品中低浓度合成甜味剂的质量控制。