Determination of a metabolite of nifursol in foodstuffs of animal origin by liquid–liquid extraction and liquid chromatography with tandem mass spectrometry

Abstract

An analytical method has been developed for the detection of a metabolite of nifursol, 3,5-dinitrosalicylic acid hydrazide, in foodstuffs of animal origin (chicken liver, pork liver, lobster, shrimp, eel, sausage, and honey). The method combines liquid chromatography and tandem mass spectrometry with liquid-liquid extraction. Samples were hydrolyzed with hydrochloric acid and derivatized with 2-nitrobenzaldehyde at 37°C for 16 h. The solutions of derivatives were adjusted to pH 7.0-7.5, and the metabolite was extracted with ethyl acetate. 3,5-Dinitrosalicylic acid hydrazide determination was performed in the negative electrospray ionization method. Both isotope-labeled internal standard and matrix-matched calibration solutions were used to correct the matrix effects. Limits of quantification were 0.5 μg/kg for all samples. The average recoveries, measured at three concentration levels (0.5, 2.0, and 10 μg/kg) were in the range of 75.8-108.4% with relative standard deviations below 9.8%. The developed method exhibits a high sensitivity and selectivity for the routine determination and confirmation of the presence of a metabolite of nifursol in foodstuffs of animal origin.

Determination of 3.5-dinitro- N’ -(5-nitrofurfurylidene) salicylic acid hydrazide in fish using immunochromatographic strip tests

“…Detection of DNSH and its toxic metabolites should be implemented for the regulation and control of these substances since DNSH is banned as a feed additive. Numerous methods, including ultra-performance liquid chromatography-tandem mass spectrometry (Zhang, Qiao, Chen, Wang, & Xia, 2016), liquid chromatography-electrospray ionization tandem mass spectrometry in poultry eggs (Barbosa et al, 2012), liquid chromatography coupled to electrospray tandem mass spectrometry in poultry muscle tissue (Verdon, Couedor, & Sanders, 2007), liquid chromatography tandem mass spectrometry (Barbosa et al, 2011;Mulder et al, 2005;Wang et al, 2017) have been used to measure DNSH levels, however, with low sensitivity and long clean up procedures. They are also time-consuming and expensive, representing sophisticated analytical methods (Isanga et al, 2017;Liu, Xu, Suryoprabowo, Song, & Kuang, 2018a, 2018b.…”

Solid-Phase Extraction and Large-Volume Sample Stacking-Capillary Electrophoresis for Determination of Tetracycline Residues in Milk

“…This improves analytical sensitivity, with the additional advantage of removing interferences [ 1 ]. Commonly employed preconcentration techniques include liquid-liquid extraction (LLE) [ 2 ], solid-phase extraction (SPE) [ 3 ], dispersive solid-phase extraction (DSPE) [ 4 ], magnetic solid-phase extraction (MSPE) [ 5 ], and quick, easy, cheap, effective, rugged, and safe (QuEChERS) [ 6 , 7 ]. These techniques are termed off-line .…”

Facile preparation of multifunctional carbon nanotube/magnetite/polyaniline nanocomposite offering a strong option for efficient solid‐phase microextraction coupled with GC–MS for the analysis of phenolic compounds

“…Several routes have been used for extraction and preconcentration of trace levels of organic pollutants in environmental water samples including LLE, cloud point extraction, SPE, SPME, LPME, floatation separation, and membrane filtration . SPME, introduced by Pawlyszyn and coworkers in 1990 , has emerged as a prevailing and new extraction and preconcentration method of volatile and semi‐volatile organic compound at trace levels from liquid, solid, and gaseous samples that possess fast diffusion rate, portable, solvent‐free, easily automated, inexpensive, and high enrichment factor properties.…”