色谱

色谱 ›› 2020, Vol. 38 ›› Issue (5): 529-537.DOI: 10.3724/SP.J.1123.2019.06030

• 研究论文 • 上一篇    下一篇

固相萃取-液相色谱-串联质谱法同时测定蜂蜜中16种黄酮类化合物和阿魏酸

侯建波1,2,*(), 谢文1,2, 钱艳3, 史颖珠3, 陆顺3, 盛涛3, 陈文彬4   

  1. 1 杭州海关技术中心, 浙江 杭州 310016
    2 浙江省检验检疫科学技术研究院, 浙江 杭州 310016
    3 浙江立德产品技术有限公司, 浙江 杭州 310016
    4 福建农林大学蜂学学院, 福建 福州 350002
  • 收稿日期:2019-06-29 出版日期:2020-05-08 发布日期:2020-12-10
  • 通讯作者: 侯建波
  • 作者简介:侯建波.Tel:057181100294, E-mail:xmuhjb@163.com
  • 基金资助:
    国家重点研发计划(2017YFF0211000);浙江出入境检验检疫局科技计划项目(ZK201710X)

Simultaneous determination of 16 flavonoids and ferulic acid in honey by solid phase extraction and high performance liquid chromatography-tandem mass spectrometry

HOU Jianbo1,2,*(), XIE Wen1,2, QIAN Yan3, SHI Yingzhu3, LU Shun3, SHENG Tao3, CHEN Wenbin4   

  1. 1 Technic Center of Hangzhou Customs, Hangzhou 310016, China
    2 Zhejiang Academy of Science and Technology for Inspection and Quarantine, Hangzhou 310016, China
    3 Zhejiang Lead Product Technic Co. Ltd., Hangzhou 310016, China
    4 College of Bee Science, Fujian Agriculture and Forestry University, Fuzhou 350002, China
  • Received:2019-06-29 Online:2020-05-08 Published:2020-12-10
  • Contact: HOU Jianbo
  • Supported by:
    National Key Research and Development Program of China(2017YFF0211000);Financial Support from Zhejiang Entry Exit Inspection and Quarantine Bureau(ZK201710X)

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摘要：

建立了固相萃取净化-液相色谱-串联质谱法（SPE-LC-MS/MS）同时测定蜂蜜中芦丁、杨梅素、桑黄素、槲皮素、柚皮素、橙皮素、木犀草素、染料木素、山柰酚、异鼠李素、芹菜素、松属素、汉黄芩素、白杨素、高良姜素、芫花素和阿魏酸含量的方法。蜂蜜经pH 2的盐酸溶液稀释，C18固相萃取柱净化，液相色谱-串联质谱法检测，外标法定量。以空白蜂蜜基质溶液配制0~200 μg/kg的系列标准溶液，线性相关系数大于0.997，方法定量限为20 μg/kg。在蜂蜜样品中进行加标水平为20、40、100 μg/kg的添加回收试验，回收率为64.5%~113%，相对标准偏差为1.4%~14.5%。该方法取样量少、操作简便、快捷，可用于蜂蜜中黄酮类化合物的测定。

关键词: 固相萃取, 高效液相色谱-串联质谱法, 黄酮类化合物, 蜂蜜

Abstract:

Flavonoids are polyphenol compounds that are widely distributed in honey; they play an important role in its antioxidant activity and aid in distinguishing various species of honey. An analytical method based on solid phase extraction and high performance liquid chromatography with tandem mass spectrometry (SPE-HPLC-MS/MS) for the simultaneous determination of rutin, myricetin, morin, quercetin, naringenin, hesperetin, luteolin, genistein, kaempferol, isorhamnetin, apigenin, pinocembrin, wogonin, chrysin, galangin, genkwanin, and ferulic acid in honey was developed and validated. The honey samples were diluted with HCl solution (pH 2) and cleaned up on a C18 column by solid phase extraction; the methanol eluent was filtered through a nylon membrane and analyzed by LC-MS/MS on an ODS-3 column (150 mm×4.6 mm, 3 μm). Quantitative detection was performed by LC-MS/MS in the multiple reaction monitoring (MRM) mode under negative electrospray ionization (ESI-) conditions. The external standard method was used for quantitation. The method validation data were obtained. The calibration standard curve solutions were prepared by honey matrix-matching; the linear range was 0-200 μg/kg, with correlation coefficients of the calibration standard curves greater than 0.997. The limits of quantification (LOQs) of this method were 20 μg/kg. The recoveries were in the range of 64.5%-113%, and the relative standard deviations were 1.4%-14.5% at three spiked levels (20, 40, and 100 μg/kg). The developed method is convenient, rapid, and effective, and it is suitable for the determination and confirmation of flavonoids in honey samples.

Key words: solid phase extraction (SPE), high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), flavonoids, honey