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高效液相色谱-串联质谱法同时测定调味品中8种人工合成甜味剂
Simultaneous determination of eight artificial sweeteners in flavorings by HPLC-MS/MS
【摘要】 目的建立一种高效液相色谱-串联质谱法(HPLC-MS/MS)同时测定调味品中8种人工合成甜味剂(安赛蜜、甜蜜素、糖精、阿斯巴甜、阿力甜、纽甜、三氯蔗糖、新橘皮苷二氢查耳酮)。方法样品用水提取,提取液用甲醇沉淀水溶性大分子化合物,离心后取上清液经过中性氧化铝固相萃取柱分离色素,采用C18色谱分离柱,以10 mmol/L甲酸铵溶液-乙腈进行梯度洗脱,电喷雾负离子模式下多反应监测(MRM)模式检测。结果线性范围分别为糖精于0.05~5μg/ml,三氯蔗糖于0.1~10μg/ml,其它甜味剂于0.01~1μg/ml,线性关系良好,r2>0.990。在3个添加水平下,样品平均回收率为82.7%~117.9%,RSD为0.6%~10.6%。甜味剂于液体及半固体基质中的检出限均为0.01~0.1 mg/kg,于固体基质中的检出限为0.1~1 mg/kg。结论本方法选择性强、灵敏度高、处理方法简单,可用于调味品中8种人工合成甜味剂的测定。
【Abstract】 Objective To establish a HPLC-MS/MS method for simultaneous determination of eight artificial sweeteners in flavorings.Methods The artificial sweeteners,including acesulfame-K,cyclamate,saccharin,aspartame,alitame,neotame,sucralose and neohesperidine dihydrochalcone were extracted with water and the water-soluble macromolecular compounds in flavorings were precipitated with methanol.The supernatant was cleaned-up using aluminum-N cartridges and separated on a C18 column using 10 mmol/L ammonium formic acid/acetonitrile as mobile phase and then detected by HPLC-MS/MS using multiple reaction monitoring(MRM) in negative ionization mode.Results The calibration curves showed a good linearity with correlation coefficients>0.990.The linear range for saccharin was 0.05-5 μg/ml,0.1-10 μg/ml for sucralose,and the other sweeteners was 0.01-1 μg/ml.The average recoveries were from 82.7% to 117.9%,and the relative standard deviations(RSD) were from 0.6% to 10.6%.The detection limits for liquid and semi-solid sweeteners were from 0.01 to 0.1 mg/kg and 0.1 to 1 mg/kg for solid sweeteners.Conclusion The method was specific,sensitive,easy,fast and suitable for the confirmation and quantification of 8 artificial sweeteners in flavorings.
【Key words】 Artificial sweetener; HPLC-MS/MS; flavoring; food additive;
- 【文献出处】 中国食品卫生杂志 ,Chinese Journal of Food Hygiene , 编辑部邮箱 ,2013年04期
- 【分类号】TS264;O657.63
- 【被引频次】17
- 【下载频次】330