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中国精品科技期刊2020 食品青年科学家峰会

超高效液相色谱-荧光法测定蜂蜜中百里香酚的残留量

钱振杰 曾羲 陈敬 赵悦 游淑珠 何咏欣 冯家望

钱振杰,曾羲,陈敬,等. 超高效液相色谱-荧光法测定蜂蜜中百里香酚的残留量[J]. 食品工业科技,2022,43(23):328−333. doi:  10.13386/j.issn1002-0306.2022070302
引用本文: 钱振杰,曾羲,陈敬,等. 超高效液相色谱-荧光法测定蜂蜜中百里香酚的残留量[J]. 食品工业科技,2022,43(23):328−333. doi:  10.13386/j.issn1002-0306.2022070302
QIAN Zhenjie, ZENG Xi, CHEN Jing, et al. Determination of Thymol in Honey by Ultra Performance Liquid Chromatography with Fluorescence Detector[J]. Science and Technology of Food Industry, 2022, 43(23): 328−333. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2022070302
Citation: QIAN Zhenjie, ZENG Xi, CHEN Jing, et al. Determination of Thymol in Honey by Ultra Performance Liquid Chromatography with Fluorescence Detector[J]. Science and Technology of Food Industry, 2022, 43(23): 328−333. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2022070302

超高效液相色谱-荧光法测定蜂蜜中百里香酚的残留量

doi: 10.13386/j.issn1002-0306.2022070302
基金项目: 珠海市重点科技项目(ZH22036201210211PWC);海关总署标准制修订计划(2020B166);广东省药品监督管理局科技创新团队项目(2019TDB04)。
详细信息
    作者简介:

    钱振杰(1979−),男,硕士,高级工程师,研究方向:食品质量安全技术研究,E-mail:qianzhenjie@hotmail.com

    通讯作者:

    曾羲(1991−),女,硕士,工程师,研究方向:食品分析检测,E-mail:lovelyzeng@126.com

  • 中图分类号: O657.7+2

Determination of Thymol in Honey by Ultra Performance Liquid Chromatography with Fluorescence Detector

  • 摘要: 建立了超高效液相色谱-荧光检测法测定蜂蜜中百里香的残留量的检验方法。用40%乙腈-水溶液提取蜂蜜中的百里香酚,经离心、上清液过滤后,以0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱,采用Accucore aQ色谱柱(150 mm×2.1 mm,2.6 μm)分离,荧光检测器检测(激发波长274 nm,发射波长297 nm),外标法定量。结果表明,百里香酚在0.01~3.00 μg/mL范围内线性关系良好,决定系数(R2)为0.9999,在蜂蜜基质中的平均加标回收率在87.4%~106.9%之间,变异系数在0.7%~7.3%之间,定量限为0.10 mg/kg。利用该方法测定了48份市售蜂蜜样品,仅有1份样品存在百里香酚残留。本研究建立的方法简单、迅速、可靠,适用于蜂蜜中百里香酚残留的批量筛查和定量测定。
  • 图  1  不同提取溶剂的回收率(n=3)

    Figure  1.  Recoveries of different solvents for thymol (n=3)

    图  2  不同净化方式的回收率(n=3)

    Figure  2.  Recoveries of different purification methods for thymol (n=3)

    图  3  4种色谱柱对酚类混合物(1.0 µg/mL)的分离色谱图

    Figure  3.  Chromatograms of 4 kinds of chromatographic column for mixed phenolic compounds at 1.0 µg/mL

    注:峰1:丹皮酚;峰2:丁香酚;峰3:异丁香酚;峰4:香芹酚;峰5:百里香酚;图4同。

    图  4  4种流动相对酚类混合物(1.0 µg/mL)的分离色谱图

    Figure  4.  Chromatograms of 4 kinds of mobile phase for mixed phenolic compounds at 1.0 µg/mL

    图  5  不同甲酸浓度下百里香酚(1.0 µg/mL)峰面积和保留时间的变化

    Figure  5.  Changes in peak area and retention time of thymol (1.0 µg/mL) at different concentrations of formic acid

    图  6  不同比例乙腈下香芹酚和百里香酚的分离度

    Figure  6.  Resolution of carvacrol and thymol in the presence of different concentrations of acetonitrile

    图  7  百里香酚的紫外吸收光谱

    Figure  7.  UV absorption spectrum of thymol

    图  8  百里香酚的荧光激发-发射光谱

    Figure  8.  Fluorescence excitation-emission spectrum of thymol

    图  9  阳性样品的色谱图

    Figure  9.  Chromatogram of positive sample

    表  1  百里香酚的线性范围、线性回归方程、决定系数、检出限和定量限

    Table  1.   Linear range, linear equation, correlation coefficients, limit of detection (LOD) and limit of quantitation (LOQ) of thymol

    线性范围
    (µg/mL)
    线性方程决定系数
    (R2)
    检出限
    (mg/kg)
    定量限
    (mg/kg)
    0.01~3.00y=1.537×107x−31960.99990.030.10
    下载: 导出CSV

    表  2  百里香酚的加标回收率和精密度(n=6)

    Table  2.   Spiked recoveries and relative standard deviations (RSDs) of thymol (n=6)

    基质种类添加浓度(mg/kg)平均加标回收率(%)精密度(%)
    雪脂莲蜜0.198.15.7
    0.898.33.2
    3096.90.8
    椴树蜜0.189.54.3
    0.8100.32.1
    3087.40.9
    玄参蜜0.1106.96.0
    0.896.42.1
    3091.11.8
    洋槐蜜0.195.25.8
    0.8103.21.3
    3089.50.8
    百花蜜0.198.87.3
    0.896.81.5
    3096.70.7
    下载: 导出CSV
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  • 收稿日期:  2022-08-01
  • 网络出版日期:  2022-10-21
  • 刊出日期:  2022-11-23

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