食品科学

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蜂胶样品乙醇提取物的UPLC-Q-TOF-MS指纹特征

刘莉敏1,郭 军1,*,米智慧1,王 竹2,向雪松2   

  1. 1.内蒙古农业大学食品科学与工程学院,内蒙古 呼和浩特 010018;
    2.中国疾病预防控制中心营养与食品安全所,北京 100050
  • 出版日期:2014-09-25 发布日期:2014-09-17
  • 通讯作者: 郭 军
  • 基金资助:

    “十二五”国家科技支撑计划项目(2012BAD33B01-6)

UPLC-Q-TOF-MS Fingerprint Profiling of Ethanol Extracts of Propolis

LIU Li-min1, GUO Jun1,*, MI Zhi-hui1, WANG Zhu2, XIANG Xue-song2   

  1. 1. College of Food Science and Engineering, Inner Mongolia Agricultural University, Huhhot 010018, China;
    2. National Institute For Nutrition and Food Safety, Chinese Center for Disease Control and Prevention, Beijing 100050, China
  • Online:2014-09-25 Published:2014-09-17
  • Contact: GUO Jun

摘要:

探索蜂胶质谱指纹在建立蜂胶品质和真实性判别模型的可行性,对9 个国内外蜂胶样品用体积分数75%热乙醇溶液提取,提取液用超高效液相色谱-四极杆飞行时间质谱联用仪进行一级阳离子化总离子流色谱和总质谱(色谱和质谱指纹)的采集分析。从总离子流图指纹发现2 个广东成品蜂胶色谱指纹与其余7 个极为不同,判断为异常蜂胶;9 个蜂胶样品均未检出芦丁和槲皮素。总离子流图指纹结合峰内分子的质荷比可直观对比蜂胶样品的相同和差异,能克服色谱峰的漂移,比单用液相色谱指纹特征判别更可靠。总质谱指纹主成分分析对2 个异常蜂胶的判别与色谱指纹结果一致,表明色谱和质谱指纹结合有望建立更稳健的蜂胶鉴别方法。

关键词: 蜂胶, 超高效液相色谱-四极杆飞行时间质谱, 色谱指纹, 质谱指纹, 主成分分析

Abstract:

This study aimed to explore a robust method for propolis authentication. Ultra high performance liquid
chromatography-quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) first grade cation electronic spray
ionization ([M+H]+) total ion chromatogram (TIC) and mass spectrometry (MS) were used to acquire and analyze
chromatographic fingerprints and mass spectral fingerprints of hot 75% (V/V) ethanol extracts of 9 propolis samples. Samples
of two brands of propolis from Guangdong province were identified as abnormal or fake propolis by TIC fingerprint profile;
neither rutin nor quercetin was found in all 9 samples. Compared to HPLC chromatographic fingerprint profiling, TIC profile
combined with m/z ratio of molecules in the peak could improve the discrimination power of chromatographic fingerprint
profiling. Through principal component analysis (PCA) of mass spectral fingerprint two abnormal propolis samples were
confirmed. This study implies that the combination of the two strategies may be helpful to develop a more accurate method
for propolis authentication. Mass spectrum contains far more information which is more complicated when compare to
chromatogram, so that deserving to be further explored.

Key words: propolis, ultra high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLCQTOF-MS), chromatographic fingerprint profiling, mass spectrum fingerprint profiling, principal component analysis (PCA)

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