Piątkowska Marta, Jedziniak Piotr, Olejnik Małgorzata, Pietruk Konrad, Żmudzki Jan, Posyniak Andrzej
Department of Pharmacology and Toxicology, National Veterinary Research Institute, 24-100, Pulawy, Poland.
J Vet Res. 2017 Sep 19;61(3):299-305. doi: 10.1515/jvetres-2017-0040. eCollection 2017 Sep.
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.
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.
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.
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.
本文介绍了采用超高效液相色谱-串联质谱技术同时测定饲料中10种非法偶氮染料的方法。
用己烷提取染料，蒸发至干后进行分析。以乙腈（A）和0.1%甲酸（B）作为流动相，采用梯度洗脱，7分钟内实现分离。
验证结果表明该方法具有可重复性，在三个浓度水平（50、500和5000 µg/kg）下进行了评估。工作范围内所有基质校准曲线均呈线性（R为0.9904至1.0），重复性在2.1%至24%之间，回收率在77.9%至120%之间。不同染料的检测限和定量限分别为1 - 2 µg/kg和5 - 10 µg/kg。此外，该方法应用于内部制备的含有苏丹红I且含量分别为0.5、5和50 mg/kg的饲料的均匀性测试。
成功开发并验证了一种灵敏、选择性好且快速的多残留方法。通过对含有苏丹红I的实验饲料的分析证实了其稳健性。
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