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当前位置: 首页 > 文章 > 高效液相色谱-质谱法测定输韩泡菜中的甜蜜素 食品科学 2012,33 (4) 186-188
Position: Home > Articles > Determination of Sodium Cyclamate in Pickles by Liquid Chromatography-Mass Spectrometry FOOD SCIENCE 2012,33 (4) 186-188

高效液相色谱-质谱法测定输韩泡菜中的甜蜜素

作  者：
徐琴;牟志春;郝杰;刘琳;蔡雪;林洪
单  位：
青岛出入境检验检疫局;山东出入境检验检疫局食品农产品检测中心;中国海洋大学食品科学与工程学院
关键词：
泡菜;甜蜜素;液相色谱-质谱法;测定
摘  要：
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。
译  名：
Determination of Sodium Cyclamate in Pickles by Liquid Chromatography-Mass Spectrometry
作  者：
XU Qin1,2,MU Zhi-chun2,HAO Jie3,LIU Lin2,CAI Xue2,LIN Hong1(1.College of Food Science and Engineering,Ocean University of China,Qingdao 266003,China; 2.Food and Agricultural Products Testing Agency,Shandong Entry-Exit Inspection and Quarantine Bureau, Qingdao 266002,China;3.Qingdao Entry-Exit Inspection and Quarantine Bureau,Qingdao 266002,China)
关键词：
pickles;sodium cyclamate;liquid chromatography-mass spectrometry;determination
摘  要：
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.

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