色谱

色谱

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱法同时测定调味料中的17种防腐剂和抗氧化剂

凌云1,2, 储晓刚2, 张峰2, 陈琦2,3, 赵云峰1, 吴永宁1*, 张晨光1   

  1. 1. 中国疾病预防控制中心, 北京 100021; 2. 中国检验检疫科学研究院, 北京 100123; 3. 陕西科技大学, 陕西 西安 710021
  • 收稿日期:2011-03-03 修回日期:2011-03-30 出版日期:2011-08-28 发布日期:2011-09-28
  • 通讯作者: 凌云
  • 基金资助:

    北京市科技计划项目(D08050200310804, D08050200310803)、财政部质检公益性行业科研项目(200910145)和国家科技支撑计划课题（2009BADB9B02）

Simultaneous determination of 17 preservatives and antioxidants in condiments using ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry

LING Yun1,2, CHU Xiaogang2, ZHANG Feng2, CHEN Qi2,3, ZHAO Yunfeng1, WU Yongning1*, ZHANG Chenguang1   

  1. 1. Chinese Centre for Disease Control and Prevention, Beijing 100021, China; 2. Chinese Academy of Inspection and Quarantine, Beijing 100123, China; 3. Shaanxi University of Science and Technology, Xi’an 710021, China
  • Received:2011-03-03 Revised:2011-03-30 Online:2011-08-28 Published:2011-09-28

PDF

654

被引次数

48

摘要： 建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定调味料中11种防腐剂和6种抗氧化剂的定性、定量分析方法。低脂肪和中等脂肪含量的调味料样品用饱和NaCl水溶液(用磷酸调pH为2～3)稀释混合均匀,然后用乙腈提取,正己烷液-液萃取净化(中等脂肪含量的样品提取液还需经C8固相萃取柱进一步的净化处理);脂肪含量高的样品先用正己烷稀释,再用饱和NaCl水溶液(用磷酸调pH为2～3)溶解样品,然后用乙腈提取,提取液进一步经C8固相萃取柱净化处理。提取液经C18反相色谱柱(150 mm×2.1 mm, 1.7μm)分离,流动相为20 mmol/L乙酸铵水溶液和乙腈,梯度洗脱,以电喷雾离子源负离子多反应监测(MRM)模式进行MS/MS检测。17种分析物在线性范围内具有较好的线性关系,相关系数r≥0.9955,其定量限(LOQ,信噪比为10)为0.05～5 mg/kg;空白样品中的添加回收率为79.7%～118%,精密度(以相对标准偏差计)为0.57%～13.1%。该方法适用于调味品中防腐剂和抗氧化剂的检测。

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关键词: 超高效液相色谱-串联质谱, 调味料, 防腐剂, 固相萃取, 抗氧化剂

Abstract: An ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) method was developed for the simultaneous determination of 11 preservatives and 6 antioxidants in condiments. The condiment sample with low fat or middle fat was diluted with saturated NaCl solution (adjusting pH to 2~3 with phosphoric acid), then extracted with acetonitrile. The extract was purified using liquid-liquid extraction with hexane, and the sample with middle fat was further purified using solid phase extraction with a C8 column. The condiment sample with high fat was diluted with hexane, then dissolved with saturated NaCl solution (adjusting pH to 2~3 with phosphoric acid), and extracted with acetonitrile. The extract was purified using solid phase extraction with a C8 column. The analysis was performed on a C18 column (150 mm×2.1 mm, 1.7 μm) using a gradient elution with the mobile phases of 20 mmol/L ammonium acetate buffer and acetonitrile, and determined by tandem mass spectrometry in negtive ESI mode under multiple reaction monitoring (MRM) mode. The method had good linearity (r≥0.9955). The limits of quantification (LOQs) (S/N=10) of 17 analytes ranged from 0.05 mg/kg to 5 mg/kg. The recoveries ranged from 79.7% to 118% at three spiked levels, the relative standard deviations (RSDs) ranged from 0.57% to 13.1%. The method can be applied for the determination of preservatives and antioxidants in condiments.