食品科学 ›› 2017, Vol. 38 ›› Issue (16): 245-250.doi: 10.7506/spkx1002-6630-201716039

• 安全检测 • 上一篇    下一篇

高效液相色谱-离子阱-飞行时间质谱法快速筛查饮料中植物源性成分

吕品,范素芳,赵勇,孙勇,张岩,马爱进   

  1. (1.河北医科大学基础医学院,河北?石家庄 050017;2. 河北省食品检验研究院 河北省食品安全重点实验室,河北?石家庄 050071;3.北京食品科学研究院,中国肉类食品综合研究中心,北京 100068;4.中国标准化研究院,北京 100191)
  • 出版日期:2017-08-25 发布日期:2017-08-18
  • 基金资助:
    “十二五”国家科技支撑计划项目(2015BAK36B03);“十三五”国家重点研发计划重点专项(2016YFF0202300);国家重大科学仪器设备开发专项(2012YQ03011110);河北省高等学校优秀青年基金项目(YQ2013018)

Rapid Screening and Confirmation of Plant-Derived Ingredients in Beverage by High Performance Liquid Chromatography-Ion Trap-Time of Flight Mass Spectrometry

Lü Pin, FAN Sufang, ZHAO Yong, SUN Yong, ZHANG Yan, MA Aijin,   

  1. (1. College of Basic Medicine, Hebei Medical University, Shijiazhuang 050017, China; 2. Hebei Food Safety Key Laboratory, Hebei Food Inspection and Research Institute, Shijiazhuang 050071, China; 3. China Meat Research Center, Beijing Academy of Food Sciences, Beijing 100068, China;4. China National Institute of Standardization, Beijing 100191, China)
  • Online:2017-08-25 Published:2017-08-18

摘要: 采用高效液相色谱-离子阱-飞行时间质谱对饮料中生物碱、皂苷和有机酸等24 种植物源性成分进行快 速筛查、定性识别和准确定量。样品经高速离心,过0.22 μm水系滤膜后,以C18色谱柱(2.1 mm×250 mm, 3.0 μm)分离,乙腈-0.1%甲酸溶液为流动相进行梯度洗脱,正、负离子模式同时扫描。结果表明,24 种化合物在 50~750 μg/L范围内呈良好的线性关系,相关系数均大于0.995。样品中各化合物的检出限(以信噪比不小于3计) 为8~20 μg/L。在3 种添加量(70、250、700 μg/L)条件下,其平均回收率为63.0%~126.6%,相对标准偏差为 4.11%~14.73%。该方法利用精确质量数匹配和自建标准库检索,实现快速筛查,并使用多级特征碎片离子进行确 证,具有快速、高效、准确等优点,适用于饮料中多种植物源性成分的快速筛查和测定。

关键词: 植物源性成分, 液相色谱-离子阱-飞行时间质谱, 生物碱, 皂苷

Abstract: A high performance liquid chromatography-ion trap-time of flight mass spectrometry method was used for rapid screening, confirmation and quantification of 24 alkaloids, saponins and organic acid in beverage. After centrifugation of samples at high speed and filtration through a 0.22 μm drainage membrane filter, the filtrate was separated on a C18 column (2.1 mm × 250 mm, 3.0 μm) using a binary solvent system composed of acetonitrile and water containing 0.1% of formic acid through gradient elution. The analysis was carried out both in the positive and negative ion modes. The results showed that good linear relationships were obtained in the range of 50–750 μg/L for all 24 compounds with correlation coefficients of higher than 0.995. The limits of detection (LOD) obtained at signal-to-background noise of 3 for all analytes were in the range of 8–20 μg/L. Average recoveries were between 63.0% and 126.6% at three spiked levels (70, 250 and 700 μg/L) with relative standard deviations (RSDs) of 4.11%–14.73%. Depending on the match of accurate mass number and retrieval in the self-built standard library, rapid screening was achieved and multistage characteristic fragments were also used for confirmation. The method, thanks to its rapidity, high efficiency, and good accuracy, could be used in the rapid screening and determination of multi-plant derived ingredients in beverage.

Key words: plant-derived ingredients, liquid chromatography-ion trap-time of flight mass spectrometry, alkaloid, saponin

中图分类号: