食品科学

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超高效液相色谱-串联质谱法同时测定蜂蜜中雷公藤红素和雷公藤次碱

雷美康1,彭 芳1,祝子铜1,丁 涛2,徐佳文1,吴晓勤1   

  1. 1.衢州出入境检验检疫局技术中心,浙江 衢州 324002;2.江苏出入境检验检疫局食品实验室,江苏 南京 210001
  • 出版日期:2015-06-25 发布日期:2015-06-12
  • 基金资助:

    浙江省公益性技术应用研究计划项目(2013C37101)

     

Determination of Triptolide and Wilforine in Honey by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

LEI Meikang1, PENG Fang1, ZHU Zitong1, DING Tao2, XU Jiawen1, WU Xiaoqin1   

  1. 1. Technology Center of Quzhou Entry-Exit Inspection and Quarantine Bureau, Quzhou 324002, China;
    2. Laboratory of Food, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China
  • Online:2015-06-25 Published:2015-06-12

摘要:

建立了一种超高效液相色谱-串联质谱同时检测蜂蜜中雷公藤红素和雷公藤次碱的快速分析方法。样品用水溶解后,乙腈盐析提取,采用Hypersil GOLD C18柱(50 mm×2.1 mm,1.9 μm)分离,电喷雾离子源正离子多反应监测模式串联质谱进行检测。结果表明:雷公藤红素和雷公藤次碱在0.01~20 ng/mL范围内具有较好的线性关系,相关系数均大于0.997。该方法定量限均为0.05 μg/kg。在0.05 μg/kg和1.0 μg/kg添加量条件下,雷公藤红素和雷公藤次碱的回收率为69.9%~101.5%,相对标准偏差均不大于10%(n=6)。本方法快速、灵敏、准确,适用于蜂蜜中雷公藤相关物质残留的定性、定量检测。

关键词: 超高效液相色谱-串联质谱, 蜂蜜, 雷公藤红素, 雷公藤次碱

Abstract:

A method based on ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS) has
been proposed for the determination of triptolide and wilforine residues in honey. The samples were dissolved in water and
extracted with acetonitril, separated on a Hypersil GOLD C18 column (50 mm × 2.1 mm, 1.9 μm) with gradient elution. The
determination was carried out with electrospray ion source under the positive mode and multiple reaction monitoring (SRM)
mode. The concentrations of triptolide and wilforine in the range of 0.01–20 ng/mL were linearly correlated to the peak area,
with correlation coefficients greater than 0.997. The limits of quantification (RSN > 10)for both triptolide and wilforine
were 0.05 μg/kg. The recoveries of triptolide and wilforine were 69.9%–101.5%, respectively, at spiked concentrations of
0.05 μg/kg and 1.0 μg/kg, with relative standard deviations (RSD, n = 6) lower than 10%. Our results indicate that the developed
method is rapid, sensitive and accurate for the qualitative and quantitative analysis of triptolide and wilforine in honey.

Key words: ultra performance liquid chromatography-tandem mass spectrometry, honey, triptolide, wilforine

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