食品科学

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功能性饮料中9 种水溶性维生素的HPLC-MS-MS同步检测技术

夏 静,俞 婧,孙 磊,张 岩*   

  1. 河北省食品质量监督检验研究院,河北 石家庄 050091
  • 出版日期:2014-06-25 发布日期:2014-07-03
  • 通讯作者: 张 岩

Simultaneous Determination of 9 Water Soluble Vitamins in Drinks by Liquid Chromatography Tandem Mass Spectrometry

XIA Jing, YU Jing, SUN Lei, ZHANG Yan*   

  1. Hebei Institute of Food Quality Supervision Inspection and Research, Shijiazhuang 050091, China
  • Online:2014-06-25 Published:2014-07-03
  • Contact: ZHANG Yan

摘要:

建立高效液相色谱-质谱法测定功能性饮料中9 种水溶性维生素的定性定量同步检测方法。样品利用Supelco C18(500 mg)固相萃取柱萃取后,采用Agilent plus C18(100 mm ×2.1 mm,3.5 μm)色谱柱进行分离;流动相为0.1%甲酸溶液和乙腈,梯度洗脱,采用电喷雾离子源多反应监测模式进行检测。结果表明,9 种水溶性维生素在10~1 000 ng/mL范围内线性关系良好(R2≥0.997),检出限在0.157~0.836 μg/L之间。在加标量为0.05、0.1 mg/L和1 mg/L水平下,待测物的平均回收率在80.11%~115.56%之间,测定结果的相对标准偏差小于10%。

关键词: 水溶性维生素, 高效液相色谱-质谱, 饮料

Abstract:

A method was established for the simultaneous determination of 9 water soluble vitamins in drinks using
high performance liquid chromatography tandem mass spectrometry interfaced with electrospray (HPLC-MS-MS). The
pretreatment procedure using solid phase extraction with Supelco C18 (500 mg) was simple. An Agilent plus C18 (2.1 mm ×
100 mm, 3.5 μm) column was used for the chromatographic separation, and gradient elution was performed with 0.1%
formic acid and acetonitrile as the mobile phase. Mass spectral acquisition was done in the positive ion mode by applying
multiple reaction monitoring. The method was validated in terms of linearity, sensitivity, repeatability, recovery and
selectivity. Satisfactory results in the majority of the cases were obtained, with practical limits of detection acceptable for
routine monitoring purposes. Average recoveries for the analytes ranged from 80.11% to 115.56% at spiking levels of 0.05,
0.1 and 1 mg/L. The intra- and inter-day precision (RSD) were both less than 10%.

Key words: water soluble vitamin, high performance liquid chromatography tandem mass spectrometry (HPLC-MS-MS), drinks

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