色谱

色谱 ›› 2012, Vol. 30 ›› Issue (09): 957-961.DOI: 10.3724/SP.J.1123.2012.04026

• 技术与应用 • 上一篇    下一篇

超高效液相色谱-串联质谱法测定果汁中的展青霉素

牛华, 冯雷*, 牛之瑞, 珠娜, 祝红昆, 王亚琴   

  1. 云南省产品质量监督检验研究院, 云南 昆明 650223
  • 收稿日期:2012-04-17 修回日期:2012-06-26 出版日期:2012-09-28 发布日期:2012-09-20
  • 通讯作者: 冯雷,硕士,高级工程师,研究方向为食品安全检测. Tel: (0871)5198437, E-mail: fenglei16@hotmail.com.
  • 基金资助:

    云南省食品安全检测科技服务平台(2009DA022)和云南省食品安全地方标准项目.

Determination of patulin in juice by ultra performance liquid chromatography-tandem mass spectrometry

NIU Hua, FENG Lei*, NIU Zhirui, ZHU Na, ZHU Hongkun, WANG Yaqin   

  1. Yunnan Institute of Product Quality Supervision and Inspection, Kunming 650223, China
  • Received:2012-04-17 Revised:2012-06-26 Online:2012-09-28 Published:2012-09-20

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摘要： 建立了超高效液相色谱-电喷雾串联三重四极杆质谱(UPLC-ESI-MS/MS)联用技术分析果汁中展青霉素的方法。浓缩果汁样品经酶解,乙酸乙酯提取,Oasis HLB固相萃取(SPE)小柱净化后(澄清果汁直接进行SPE净化),以C18色谱柱为分离柱,以水和乙腈作为流动相进行梯度洗脱,电喷雾离子源电离、负离子多反应监测模式质谱进行定性和定量分析。展青霉素在1.0～500.0 μg/L质量浓度范围内线性关系良好,相关系数为0.999,方法的定量限为5.0 μg/kg；加标水平为5.0、25.0和100.0 μg/kg时,加标回收率为80.6%～91.8%,相对标准偏差为1.5%～7.3%。实验结果表明,该方法简单、灵敏、准确,各项技术指标均满足国内外法规要求,可用于果汁中展青霉素的检测。

关键词: 超高效液相色谱-串联质谱, 固相萃取, 果汁, 展青霉素

Abstract: A method was developed for the simultaneous determination of patulin in juice by solid phase extraction (SPE)-ultra performance liquid chromatography coupled with electro-spray ionization tandem mass spectrometry (UPLC-ESI-MS/MS). The cloudy juice was hydrolyzed by enzyme and extracted by ethyl acetate. The extract of cloudy juice was then enriched and purified by an HLB SPE cartridge. If the juice was clear it was directly treated by the cartridge as above．The separation was performed on a C18 column with the gradient elution of acetonitrile and water. The patulin was detected by MS with electrospray negative ionization (ESI~) in the mode of multiple reaction monitoring (MRM). The good linearity was observed in the range of 1.0~500 μg/L with the correlation coefficient of 0.999 and the limit of quantitation of 5.0 μg/kg. The recoveries were in the range of 80.6%~91.8% at three spiked levels of 5.0, 25.0 and 100.0 μg/kg with the relative standard deviations of 1.5%~7.3%. It was proved to be a simple, reliable and accurate method which can fully meet the requirements of patulin detection in juice samples according to most domestic and international legislations.

Key words: juice, patulin, solid phase extraction (SPE), ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)