Chinese Journal of Chromatography

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Determination of 14 mycotoxins in Chinese herbs by liquid chromatography-tandem mass spectrometry with immunoaffinity purification

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  1. Tianjin Entry & Exit Inspection and Quarantine Bureau, Tianjin 300461, China
  • Received:2011-01-20 Revised:2011-02-25 Online:2011-06-28 Published:2011-07-25

Abstract: A method was developed for the determination of 14 mycotoxins, aflatoxins, T-2, HT-2, fumonisins, ochratoxin A, zearalenone, etc. in Chinese herbs by liquid chromatography-tandem quadrupole mass spectrometry (LC-MS/MS). The sample was extracted with phosphate buffer solution (PBS) and methanol in turn, and then purified by a high selective multifunctional immunoaffinity column. The column was washed by PBS (containing 0.1% Twain) and water, and then eluted by methanol. The eluate was dried under nitrogen, dissolved in methanol-10 mmol/L NH4Ac (40:60, v/v) solution. The mycotoxins were separated on a Waters Xterra C18 MS column (100 mm×2.1 mm, 3.5 μm) and detected by MS/MS. The limits of quantification (LOQs) of the 14 mycotoxins were from 1.0 to 5.0 μg/kg. The average recoveries of the 14 mycotoxins spiked in Chinese herbs (Ginseng, Campanulaceae, Radix and Ophiopogonis) ranged from 71.9% to 99.7% at the three spiked levels of 1.0, 5.0, 10.0 μg/kg, and the relative standard deviations (RSDs, n=6) were between 4.8% and 15.8%. The method is rapid, sensitive and accurate, and suitable for the determination of the 14 mycotoxins in Chinese medicines. The quantification limits of aflatoxins can meet the domestic and foreign requirements.

Key words: Chinese herbs, mycotoxins, immunoaffinity column purification, liquid chromatography-tandem mass spectrometry (LC-MS/MS)