高效液相色谱-质谱法测定输韩泡菜中的甜蜜素

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

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。

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 tam） 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 [M-Na]- ion ndz 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 CLOQ） 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 simole, accurate and suitable for the determination of sodium cyclamate in vickles.