超高压液相色谱-质谱法测定水果中添加的3种人工合成甜味剂

Determination of three synthetic sweeteners in fruits by ultra pressure liquid chromatography-mass spectrometry

中文关键词:  超高压液相色谱-串联质谱  甜蜜素  糖精钠  安赛蜜  水果

英文关键词:ultra-high pressure liquid chromatography-mass spectrometry  sodium cyclamate  saccharin sodium  acesulfame  fruits

中文摘要:

      目的 建立水果中3 种人工合成甜味剂(甜蜜素、糖精钠、安赛蜜)的超高压液相色谱-串联质谱 (UPLC-MS/MS)检测方法。方法 以反相C18 柱为色谱柱, 乙腈?0.02 mol/L 乙酸铵溶液为流动相, 样品经纯水 提取后用色谱柱进行分离, 串联质谱负离子多反应监测(MRM)模式测定。结果 3 种人工合成甜味剂在10~600 μg/L 范围内响应峰面积和样品质量浓度之间有良好的线性关系(相关系数r≥0.995); 甜蜜素、糖精钠和安赛蜜 的最低检出限分别为0.8、5.0、1.0 μg/kg; 在2 种添加水平下, 样品平均回收率为74.9%~111.2%, 相对标准偏 差<8%。结论 该方法前处理简单, 分析时间短, 具有良好的灵敏度和准确性, 可用于水果中甜蜜素、糖精钠、 安赛蜜的同时检测。

英文摘要:

      Objective To establish a method for the determination of three synthetic sweeteners(sodium cyclamate, saccharin sodium, and acesulfame) in fruits by ultra-high pressure liquid chromatography-mass spectrometry (UPLC-MS/MS). Methods The synthetic sweeteners were extracted with water, separated on a reversed phase C18 column using acetonitrile-0.02mol/L ammonium acetate as mobile phase, and then detected by UPLC-MS/MS under multiple reaction monitoring (MRM) mode. Results The method showed a good linearity for all the analysts over the range of 10~600 μg/L with r≥0.995. The detection limits of sodium cyclamate, saccharin sodium and acesulfame were 0.8, 5.0 μg/kg and 1.0 μg/kg, respectively. The recoveries ranged from 74.9% to 111.2% at two spiked concentrations with the relative standard deviations lower than 8%. Conclusion This established method has the advantages of easy to operate, fast to perform, with high sensitivity and accuracy, and it is suitable for detection of sodium cyclamate, saccharin sodium and acesulfame in fruits.