Chinese Journal of Chromatography

Chinese Journal of Chromatography ›› 2017, Vol. 35 ›› Issue (4): 398-404.DOI: 10.3724/SP.J.1123.2016.10042

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Determination of dimethyl yellow in foods by liquid chromatography-tandem mass spectrometry coupled with solid phase extraction

LI You1, XU Dunming2, YI Xionghai1, SHENG Yonggang1, SHI Yiyin1, ZHAO Shanzhen1, DENG Xiaojun1   

  1. 1. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China;
    2. Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361026, China
  • Received:2016-10-19 Online:2017-04-08 Published:2013-07-30
  • Supported by:

    National Key Scientific Instrument Development Project (No. 2013YQ15055705); Shanghai Technical Barrier Trade Item (Nos. 14TBT006, 15TBT004, 15TBT005); Technical Standard Item of Shanghai Science and Technology Commission (No. 15DZ0503201); Yangtze River Delta Science and Technology Cooperation Project (No. 15395810100).

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Abstract:

A liquid chromatography-tandem mass spectrometry (LC-MS/MS) was established for the determination of dimethyl yellow (DMY) in foods. The samples spiked with D5-dimethyl yellow (D5-DMY) as the internal standard were extracted with ethyl acetate, cleaned up by a ProElut DMY SPE column. The separation was performed on an XDB-C18 column (50 mm×4.6 mm, 1.8 μm) with the mobile phases of 5 mmol/L ammonium acetate aqueous solution containing 0.1% (v/v) formic acid and acetonitrile containing 0.1% (v/v) formic acid. The identification and quantitation of DMY was performed by MS/MS in positive electrospray ionization (ESI+) and multiple reaction monitoring (MRM) mode. The quantitative analysis was carried out by internal standard method. A good linear relationship, with the correlation coefficient (r2) greater than 0.999, was found in the mass concentration range of 0-50 μg/L. The limit of detection (LOD, S/N>3) and the limit of quantitation (LOQ, S/N>10) were 2 μg/kg and 10 μg/kg, respectively. The recoveries of DMY in foods spiked with 10, 20 and 100 μg/kg varied from 93.3% to 98.9%, and the relative standard deviations (RSDs) were between 1.6% and 3.9% (n=6). The method can effectively correct the ionization suppression, and it is sensitive, accurate and suitable for the monitoring of DMY in sufu, chili sauce, egg, dried bean curd, candy and ham.

Key words: dimethyl yellow (DMY), foods, internal standard method, liquid chromatography-tandem mass spectrometry (LC-MS/MS), matrix effect (ME), solid phase extraction (SPE)

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