高效液相色谱-质谱法测定输韩泡菜中的甜蜜素

建立输韩泡菜中禁用甜味剂甜蜜素的高效液相色谱-质谱测定方法。泡菜样品用水提取,离心后采用液相色谱柱分离,质谱检测器检测,外标法定量。色谱条件:Agilent ZORBAX SB-C18柱(4.6mm×250mm,5μm),流动相:乙腈-体积分数0.1%甲酸溶液(25:75,V/V),流速0.6mL/min。采用负离子模式的电喷雾质谱检测,以特征离子峰M-Na]-m/z 178.1进行选择性离子分析检测,对实验条件进行优化,线性范围为0.1～5.0mg/kg,相关系数R2为0.99987,定量检测限为0.1mg/kg。添加标准回收实验表明:本方法在添加水平分别为0.10、0.15mg/kg和0.20mg/kg时样品平均回收率在82.0%～97.3%之间,相对标准偏差在2.59%～4.82%之间(n=6),说明本方法准确可靠。

Determination of Sodium Cyclamate in Pickles by Liquid Chromatography-Mass Spectrometry

A liquid chromatography-mass spectrometry(LC-MS) method was developed for determining sodium cyclamate in pickles.Pickle samples were extracted directly by water and the separation was performed on a ZORBAX SB-C18 column(4.6 mm × 250 mm,5 μm) in an isocratic elution mode using a mobile phase consisting of acetonitrile and 0.1% formic acid(25:75,V/V) at a flow rate of 0.6 mL/min.Sodium cyclamate was monitored by ESI MS in the SIM negative ion mode on the basis of -ion m/z 178.1 and quantified using the external standard method.Key experimental conditions were optimized.The calibration curve of the method revealed an excellent linear relationship in the concentration range of 0.1-5.0 mg/kg(R2 =0.99987),and the limit of quantification(LOQ) was 0.1 mg/kg.The recovery rates across three spike levels were higher than 82.0% with RSD of 2.59%-4.82%(n = 6).The method was simple,accurate and suitable for the determination of sodium cyclamate in pickles.