食品科学

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QuEChERS-超高效液相色谱-串联质谱法快速测定饮料中13 种饱和内酯类合成香料

王玉健1,纪少凡1,陈文慧1,黄惠玲1,董存柱2,*   

  1. 1.海南出入境检验检疫局检验检疫技术中心,海南 海口 570311;2.海南大学环境与植物保护学院,海南 海口 570228
  • 出版日期:2016-06-25 发布日期:2016-06-29
  • 通讯作者: 董存柱
  • 基金资助:

    国家质检总局科技计划项目(2013IK153);海南省重点科技计划项目(ZDXM2014083);
    国家自然科学基金青年科学基金项目(31360447);海南省自然科学基金项目(212018;313105)

Rapid Determination of 13 Synthetic Saturated Lactones Added as Flavors in Beverage by QuEChERS Method Coupled with Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

WANG Yujian1, JI Shaofan1, CHEN Wenhui1, HUANG Huiling1, DONG Cunzhu2,*   

  1. 1. Inspection and Quarantine Technology Center, Hainan Entry-Exit Inspection and Quarantine Bureau, Haikou 570311, China;
    2. College of Environment and Plant Protection, Hainan University, Haikou 570228, China
  • Online:2016-06-25 Published:2016-06-29
  • Contact: DONG Cunzhu

摘要:

建立超高效液相色谱-串联质谱法快速测定饮料中13 种饱和内酯类合成香料的方法。采用QuEChERS前处理法,以乙腈提取,N-丙基乙二胺填料吸附剂直接净化,电喷雾离子源、多反应监测正离子模式扫描,外标法定量。13 种饱和内酯在0.025~0.50 μg/mL范围内质量浓度与峰面积呈良好的线性关系,仪器检出限为0.025 μg/mL,方法的检出限为0.10 mg/kg,定量限为0.40 mg/kg,添加量为0.10、0.20、0.40 mg/kg时13 种饱和内酯的平均回收率范围分别为88.5%~103%,相对标准偏差为3.8%~11%(n=10)。本方法可用于饮料中饱和内酯类化合物的快速定性、定量检测。

关键词: 饱和内酯类香料, 饮料, QuEChERS, 超高效液相色谱-串联质谱

Abstract:

method for determining 13 synthetic saturated lactones added as flavors in beverage by ultra performance
liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established. The target compounds were
extracted with acetonitrile and determined by quick easy cheap effective rugged and safe (QuEChERS) pretreatment
coupled with UPLC-MS/MS (under MRM mode) with an external standard method. The limits of detection (LODs) were
0.025 μg/mL for the instrument and 0.10 mg/kg for the method, respectively. The limit of quantitation (LOQ) was
0.40 mg/kg for the method. The average recoveries of 13 lactones were between 88.5% and 103% at spiked levels of 0.10,
0.20 and 0.40 mg/kg with relative standard derivation (RSDs) of 3.8%–11% (n = 10). The method was reliable and allowed
simultaneous quantitative determination of saturated lactones in beverage.

Key words: saturated lactones, beverage, QuEChERS, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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