食品科学 ›› 2012, Vol. 33 ›› Issue (4): 186-188.doi: 10.7506/spkx1002-6630-201204038

• 分析检测 • 上一篇    下一篇

高效液相色谱-质谱法测定输韩泡菜中的甜蜜素

徐 琴,牟志春,郝 杰,刘 琳,蔡 雪,林 洪   

  1. 1.中国海洋大学食品科学与工程学院 2.山东出入境检验检疫局食品农产品检测中心 3.青岛出入境检验检疫局
  • 出版日期:2012-02-25 发布日期:2012-02-14

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

XU Qin,MU Zhi-chun,HAO Jie,LIU Lin,CAI Xue,LIN Hong   

  1. 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
  • Online:2012-02-25 Published:2012-02-14

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。

关键词: 泡菜, 甜蜜素, 液相色谱-质谱法, 测定

Abstract: 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 [M-Na]-  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.

Key words: pickles, sodium cyclamate, liquid chromatography-mass spectrometry, determination

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