色谱

色谱 ›› 2010, Vol. 28 ›› Issue (12): 1128-1131.DOI: 10.3724/SP.J.1123.2010.01128

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱法同时测定浓缩苹果汁中的4种链格孢霉毒素

何强*, 李建华, 孔祥虹, 乐爱山, 吴双民   

  1. 陕西出入境检验检疫局检验检疫技术中心, 陕西 西安 710068
  • 收稿日期:2010-09-03 修回日期:2010-10-22 出版日期:2010-12-28 发布日期:2010-08-28
  • 通讯作者: 何强,工程师,主要从事农兽药残留检测研究. Tel: (029)85407235, E-mail: heq@snciq.gov.cn.
  • 基金资助:

    国家质量检验公益性科研项目(200810618)和陕西省农业科技攻关项目(2010k01-19).

Simultaneous determination of four Alternaria toxins in apple juice concentrate by ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry

HE Qiang*, LI Jianhua, KONG Xianghong, YUE Aishan, WU Shuangmin   

  1. Inspection and Quarantine Technology Centre, Shaanxi Entry-Exit Inspection and Quarantine Bureau, Xi’an 710068, China
  • Received:2010-09-03 Revised:2010-10-22 Online:2010-12-28 Published:2010-08-28
  • Contact: HE Qiang

PDF

737

被引次数

47

摘要： 建立了浓缩苹果汁中链格孢霉素、链格孢酚、腾毒素、链格孢酚甲醚4种毒素残留量的固相萃取-超高效液相色谱-串联质谱检测方法。样品用水稀释后,用PS DVB固相萃取柱净化,外标法定量。测定时用BEH C18色谱柱(50 mm×2.1 mm, 1.7 μm)分离,乙腈和水梯度洗脱,质谱测定采用多反应监测(MRM)模式。4种链格孢霉毒素的测定低限在1.0～5.0 μg/L范围内,加标回收率为77.8%～117.2%,相对标准偏差均低于9.7%。该方法灵敏、稳定、可靠,可用于浓缩苹果汁样品中4种链格孢霉毒素的检测和确证。

关键词: 超高效液相色谱-串联质谱法, 链格孢酚, 链格孢酚甲醚, 链格孢霉素, 浓缩苹果汁, 腾毒素

Abstract: An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of altenuene (ALT), alternariol (AOH), tentoxin and alternariol monomethyl ether (AME) in apple juice concentrate (AJC). The sample was diluted with water, and then cleaned up with a PS DVB column. The quantification was carried out using an external standard method. The UPLC was performed on a BEH C18 column (50 mm×2.1 mm, 1.7 μm) using a gradient elution of acetonitrile and water. The MS/MS was performed with multiple reaction monitoring (MRM) mode. The limits of quantification of the four Alternaria toxins were between 1.0 and 5.0 μg/L. The recoveries were 77.8%~117.2% with the relative standard deviations less than 9.7%. The method is sensitive, stable and reliable. It’s suitable for the quantitative and qualitative analyses of the four Alternaria toxins in AJC.

Key words: altenuene, alternariol, alternariol monomethyl ether, apple juice concentrate, tentoxin, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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