液相色谱-串联质谱法同时测定食品中9种甜味剂

建立了高效液相色谱-串联质谱法同时测定食品中9种甜味剂(安赛蜜、糖精钠、甜蜜素、阿斯巴甜、三氯蔗糖、阿力甜、甜菊糖苷、爱德万甜和纽甜)含量的分析方法。样品经超声、离心等前处理后过0.22μm滤膜后上机分析。采用AQ-C18(100 mm×2.1 mm×3μm)为分离柱,c(乙酸铵)为20 mmol/L的水溶液-φ(甲酸)为0.1%的乙腈溶液为流动相,梯度洗脱,在ESI负离子模式下,采用多反应监测模式进行测定,以质量数和保留时间定性、峰面积定量。结果表明,9种甜味剂在工作曲线范围内相关系数均大于0.9990,方法检出限在0.020~0.055 mg/kg,食品加标回收率为90.6%~111.5%,其相对标准偏差(n=6)均小于6.0%。应用此方法对食品(白酒、饮料、果冻、酸奶、糖果)中9种甜味剂进行检测,前处理步骤简单,测定快速、准确度和灵敏度高,能满足国家标准对食品中9种甜味剂的分析要求,与国家标准方法相比,提高了分析效率。

Simultaneous Determination of Nine Sweeteners in Food by Liquid Chromatography-Tandem Mass Spectrometry

A HPLC-MS/MS method was established for simultaneous determination of nine sweeteners in foods(acesulfame K,saccharin sodium,sodium cyclamate,aspartame,sucralose,alitame,stevioside,advantame and neotame).After ultrasound and centrifugation,the samples were filtered through 0.22μm membrane and then separated with AQ-C18 column(100 mm×2.1 mm×3μm)using 20 mmol/L ammonium acetate solution and 0.1%formic acid acetonitrile solution as mobile phase and gradient elution were carried out.Under ESI negative ion mode,multiple reaction monitoring mode was used to qualitatively determine the mass number,retention time,and quantitatively measure the peak area.The results demonstrated that the calibration curves of nine sweeteners were good linearity for sweeteners with correlation coefficients of 0.9990.The limits of quantification of the nine sweeteners were 0.020-0.055 mg/kg.The adding standard recovery rate was 90.6%-111.5%,and the relative standard deviation was less than 6.0%(n=6).This method had the advantages including simple pretreatment,fast measurement and high accuracy and sensitivity,which was suitable for qualitative and quantitative measurement of 9 sweeteners in food(beverages,yogurt,jelly,candies and wines),and also met and greatly improved the requirements of national standard.