食品与发酵工业 >

2021 , Vol. 47 >Issue 12: 250 - 256

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.025865

分析与检测

超高效液相色谱-串联质谱法测定蜂蜜中五种水溶性维生素的含量

  • 薛霞 ,
  • 赵慧男 ,
  • 魏莉莉 ,
  • 丁一 ,
  • 宿书芳 ,
  • 卢兰香 ,
  • 王骏 ,
  • 刘艳明 ,
  • 胡梅
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  • 1(山东省食品药品检验研究院,山东 济南, 250101)
    2(山东省食品药品安全检测工程技术研究中心,山东 济南, 250101)
硕士,研究员(刘艳明研究员为通讯作者,E-mail:msymliu@163.com)

收稿日期: 2020-10-12

  修回日期: 2020-11-17

  网络出版日期: 2021-07-22

基金资助

山东省自然科学基金项目(ZR2017MC069)

收起

Determination of five water-soluble vitamins in honey by ultra performance liquid chromatography-tandem mass spectrometry

  • XUE Xia ,
  • ZHAO Huinan ,
  • WEI Lili ,
  • DING Yi ,
  • SU Shufang ,
  • LU Lanxiang ,
  • WANG Jun ,
  • LIU Yanming ,
  • HU Mei
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  • 1(Shandong Institute for Food and Drug Control,Jinan 250101,China)
    2(Shandong Research Center of Engineering and Technology for Safety Inspection of Food and Drug,Jinan 250101,China)

Received date: 2020-10-12

  Revised date: 2020-11-17

  Online published: 2021-07-22

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摘要

建立了蜂蜜中维生素B1、维生素B2、维生素B5(泛酸)、维生素B6(吡哆醇)和维生素B7(生物素)同时测定的超高效液相色谱-串联质谱的分析方法。样品经20 mmol/L甲酸铵溶液提取,HLB固相萃取柱净化,采用HSS T3色谱柱分离,以甲醇和20 mmol/L甲酸铵为流动相进行梯度洗脱,采用电喷雾离子源正离子模式,多反应监测进行检测,外标法定量。该方法在5~200 ng/mL范围内线性关系良好(R2＞0.99),5种维生素检出限均为20 μg/kg,定量限均为50 μg/kg。在空白蜂蜜样品中进行50、250、500 μg/kg 这3个水平的加标回收实验,方法的平均回收率为90.2%~108.8%,精密度小于15%。该方法简便、高效、准确性好、抗干扰能力强,可用于蜂蜜中5种水溶性维生素的同时检测。

关键词： 蜂蜜; 水溶性维生素; 超高效液相色谱-串联质谱法; 固相萃取柱

本文引用格式

薛霞 , 赵慧男 , 魏莉莉 , 丁一 , 宿书芳 , 卢兰香 , 王骏 , 刘艳明 , 胡梅 . 超高效液相色谱-串联质谱法测定蜂蜜中五种水溶性维生素的含量[J]. 食品与发酵工业, 2021 , 47(12) : 250 -256 . DOI: 10.13995/j.cnki.11-1802/ts.025865

Abstract

An ultra performance liquid chromatography coupled with tandem-mass spectrometric (UPLC-MS/MS) method was developed for simultaneous determination of thiamine (B1), riboflavin (B2), pantothenic acid (B5), pyridoxine (B6), and biotin (B7) in honey. The samples were extracted with 20 mmol/L ammonium formate solution, and cleaned-up with a HLB solid phase extraction (SPE) column. The extracts were separated on a HSS T3 column with a gradient elution using methanol and 20 mmol/L ammonium formate as mobile phases. Mass spectral acquisition was performed in the positive ion mode by applying multiple reaction monitoring (MRM) with external standard method. The results showed that five water-soluble vitamins showed good linearities in the range of 5-200 ng/mL with correlation coefficients 0.99. The limits of detection(LODs) and limits of quantification (LOQs) for the five water-soluble vitamins were 20 μg/kg and 50 μg/kg respectively. The recoveries of analytes from blank honey at three levels of 50,250 and 500 μg/kg ranged from 90.2% to 108.8% with relative standard deviations less than 15%. This rapid and sensitive method is suitable for the determination of five water-soluble vitamins in honey.

Key words： honey; water-soluble vitamins; ultra performance liquid chromatography coupled with tandem-mass spectrometry; solid phase extraction

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