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Chemical Research in Chinese Universities ›› 2012, Vol. 28 ›› Issue (5): 797-801 .

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Stable Isotope Dilution Analysis of Gibberellin Residues in Tomato Paste by Liquid Chromatography-Tandem Mass Spectrometry

SUN Li1, ZHAO Yan-sheng1,2, NIE Xue-mei1, LING Yun1, CHU Xiao-gang1, SHANG De-jun3, DONG Ying2   

  1. 1. Institute of Food Safety, Chinese Academy of Inspection and Quarantine, Beijing 100123, P. R. China;
    2. School of Food and Biological Engineering, Jiangsu University, Zhenjiang 212013, P. R. China;
    3. Xinjiang Extry-exit Inspection and Quarantine Bureau, Urumqi 830063, P. R. China
  • Received:2012-03-19 Revised:2012-06-11 Online:2012-09-25 Published:2012-09-07
  • Supported by:
    Supported by the Project of Chinese Academy of Inspection and Quanrantine(No.2010JK001) and the Project of Xinjiang Entry-exit Inspection and Quarantine Bureau, China(No.2010XK0033).

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Abstract: An accurate and sensitive method for the simultaneous determination of gibberellic acid(GA3), gibberellin A4(GA4) and gibberellin A7(GA7) residues in tomato paste was developed by coupling solid phase extraction to high performance liquid chromatography-tandem mass spectrometry(LC-MS/MS) with electrospray ionization based stable isotope dilution analysis(SIDA). The isotope labeled internal standard can compensate for the losses during the extraction and cleanup steps and for discrimination due to ion suppression. After extraction from methanol, hydrophile lipophilic balance(HLB) solid phase extraction(SPE) column was tested for the capacity of the cleanup of the tomato paste in compared with C18 SPE column which is the common way to the detection of GAs, and the former gained better result. Spiked experiments were performed in the non-contaminated tomato pastes and the recoveries of GA3, GA4 and GA7 were 42.6%―75.0% in external standard method(ESM) and 91.1%―103.8% in internal standard method(ISM) respectively. The validities of this method were investigated and good analytical performance for the three GAs was obtained, including low limits of method detection(2 ng/g for GA3 and GA4, 0.3 ng/g for GA7), excellent linear dynamic ranges(5―500 ng/g for GA3 and GA4, 1―100 ng/g for GA7) and good relative standard deviation ranges(4.8%―9.4% for the intra-day test and 3.5%―11.9% for the inter-day test).

Key words: Gibberellin, Tomato paste, Liquid chromatography-tandem mass spectrometry(LC-MS/MS), Stable isotope dilution analysis(SIDA)