Citation: XUE SUN, XI Cun-Xian, TANG Bo-Bin, WANG Guo-Min, CHEN Dong-Dong, ZHAO Hua. Determination of Aflatoxins and Zeranols in Animal-Originated Foods by High Performance Liquid Chromatography-Tandem Mass Spectrometry Combined With Immunoaffinity Clean-up Column[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(6): 970-978. doi: 10.11895/j.issn.0253-3820.150229 shu

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

XUE SUN ^1,2, ,
XI Cun-Xian ³ ,
TANG Bo-Bin ³ ,
WANG Guo-Min ³ ,
CHEN Dong-Dong ⁴ ,
ZHAO Hua ²

1.
Department of Pharmacy, People's Hospital of the Tibet Autonomous Region, Lhasa 850000, China;
2.
College of Pharmacy, Chongqing medical University, Chongqing 400016, China;
3.
Chongqing Entry-Exit Inspection and Quarantine Bureau, Chongqing 400020, China;
4.
Chinese Academy of Inspection and Quarantine, Beijing 100123, China

Received Date: 22 July 2015
Revised Date: 12 April 2016

Figures(2)

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.
- Animal-originated foods,
- Combination immunoaffinity column,
- Aflatoxins,
- Zeranols,
- High performance liquid chromatography-tandem mass spectrometry
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