Simultaneous Determination of Ten Illegal Azo Dyes in Feed by Ultra-high Performance Liquid Chromatography Tandem Mass Spectrometry.

INTRODUCTION

The paper presents the method of simultaneous determination of 10 illegal azo dyes in feed by ultra-high performance liquid chromatography coupled with tandem mass spectrometry technique.

MATERIAL AND METHODS

The dyes were extracted with hexane, evaporated to dryness, and analysed. Separation was achieved in 7 min in a gradient elution using acetonitrile (A) and 0.1% formic acid (B) as a mobile phase.

RESULTS

The validation results showed the repeatability of the method, which was evaluated at three levels (50, 500, and 5,000 µg/kg). All the matrix calibration curves for the working ranges were linear (R 0.9904 to 1.0), the repeatability was between 2.1% and 24%, and recoveries ranged from 77.9% to 120%. The LOD and LOQ were at 1-2 and 5-10 µg/kg for different dyes, respectively. Furthermore, the method was applied in the homogeneity tests of the in-house prepared feed containing Sudan I at the levels of 0.5, 5, and 50 mg/kg.

CONCLUSIONS

A sensitive, selective, and fast multiresidue method was successfully developed and validated. Its robustness was confirmed by the analysis of an experimental feed containing Sudan I.