Determination of Aflatoxins and Zeranols in Animal-Originated Foods by High Performance Liquid Chromatography-Tandem Mass Spectrometry Combined With Immunoaffinity Clean-up Column / 分析化学

A high performance liquid chromatography-tandem mass spectrometric ( HPLC-MS / MS) method coupled with an immunoaffinity clean-up column was successfully developed for determination of aflatoxins (AFB1 , AFB2 , AFG1 , AFG2 , AFM1 and AFM2 ) and zeranols ( α-zeranol, β-zeranol, α-zearalenol,β-zearalenol, zearalanone and zearalenone ). The sample was extracted with methanol-acetonitrile (20∶ 80, V/ V) after enzymatic digestion by β-glucuronidase / sulfatase, and the extraction solution was passed through glassy fiber filter paper and then diluted with phosphate buffer solution (PBS). The reconstituted solution was cleaned up with IAC-AZ immunoaffinity column, and then analyzed by HPLC-MS / MS in multiple reaction monitoring (MRM) mode. The results indicated that the linear detection range was 0. 03-6. 0 μg / L for AFB2 and AFG2 , and 0. 05-20 μg / L for the rest compounds. The correlation coefficients were above 0. 999. The limits of detection (LOD) and limits of quantitation (LOQ) were 0. 01-0. 03 μg / kg and 0. 04-0. 09 μg / kg, respectively. The recoveries of the aflatoxins and zeranols were in the range of 73. 6% -98. 4% at the spiked levels of 0. 5, 1 and 5 μg / kg, and the relative standard deviations (RSDs) were in the range of 1. 9% -11. 2% . The method was proved to be simple and accurate, and suitable for the rapid determination of aflatoxins and zeranols in animal-originated foods.

Determination of Zeranols in Plant Tissue by Rapid Resolution Liquid Chromatography-Mass Spectrometry/Mass Spectrometry / 分析化学

A method was developed for the determination of zeranols (α,β-zearalanol,α,β-zearalenol,zear-alanone,zearalenone) with RRLC-MS/MS in the plant tissue. The samples were extracted with acetonitrile and reextracted with aqueous alkaline solution,cleaned up with MAX column and then determined by RRLC-MS/MS using multiple reaction monitoring ( MRM) scan mode. The results showed that the working curves were linear in the range of 0 -20 μg/kg. The limits of detection ( LOD) of zeranols were 0.5 μg/kg and the limits of quantification (LOQ) was 1. 0μg/kg. Extraction recoveries for zeranols ranged from 75. 8% to 105.4% and RSD was between 2.4% and 12.1%. The method is suitable for the determination of zeranols in the plant tissue.