scholarly journals Development and Validation of Confirmatory Method for Analysis of Nitrofuran Metabolites in Milk, Honey, Poultry Meat and Fish by Liquid Chromatography-Mass Spectrometry

2016 ◽  
Vol 39 (1) ◽  
pp. 15-22 ◽  
Author(s):  
Fatih Alkan ◽  
Arzu Kotan ◽  
Nurullah Ozdemir
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Solid Phase ◽  
Poultry Meat ◽  
Fish Samples ◽  
Low Levels ◽  
Reported Data ◽  
Development And Validation ◽  
Nitrofuran Metabolites

AbstractIn this study we have devoloped and validated a confirmatory analysis method for nitrofuran metabolites, which is in accordance with European Commission Decision 2002/657/EC requirements. Nitrofuran metabolites in honey, milk, poultry meat and fish samples were acidic hydrolised followed by derivatisation with nitrobenzaldehyde and liquid-liquid extracted with ethylacetate. The quantitative and confirmative determination of nitrofuran metbolites was performed by liquid chromatography/electrospray ionisation tandem mass spectrometry (LC/ESI-MS/MS) in the positive ion mode. In-house method validation was performed and reported data of validation (specificity, linearity, recovery, CCα and CCβ). The advantage of this method is that it avoids the use of clean-up by Solid-Phase Extraction (SPE). Furthermore, low levels of nitrofuran metabolites are detectable and quantitatively confirmed at a rapid rate in all samples.

scholarly journals Simultaneous Determination of Malachite Green, Chloramphenicols, Sulfonamides, and Fluoroquinolones Residues in Fish by Liquid Chromatography-Mass Spectrometry

2020 ◽  
Vol 2020 ◽  
pp. 1-12
Author(s):  
Yongping Chen ◽  
Sudong Xia ◽  
Xianqin Han ◽  
Zhiru Fu
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Formic Acid ◽  
Simultaneous Determination ◽  
Mobile Phase ◽  
Solid Phase ◽  
Hydrophilic Lipophilic Balance ◽  
Relative Standard ◽  
Fish Samples

A fast-analytical method using simplified extraction has been developed for the simultaneous determination of 42 compounds from 4 different classes of veterinary drugs (amphenicols, triphenylmethane, fluoroquinolones, and sulfonamides) in fish by reverse phase liquid chromatography-tandem mass spectrometry. The selection of extraction reagents was optimized using different types of microfiltration membrane, mobile phase, and LC column. Samples were extracted using 0.4% hydrochloric acid in acetonitrile and ethyl acetate and then were cleaned up using solid-phase extraction Cleanert Alumina N columns (500 mg) and Oasis hydrophilic-lipophilic balance (HLB) cartridges. The chromatographic separation was performed on a XR-ODS C8 column using a mobile phase of (A) 0.1% formic acid and 2 mM ammonium acetate and (B) 0.1% formic acid acetonitrile at a flow rate of 0.25 mL·min−1. The results indicated 67.7–112.8% recovery of 42 compounds with an intra- and interday relative standard deviations less than 10%. The limits of quantification for analytes were in the range of 0.3–1.0 μg kg−1 for samples which were satisfactory to support future surveillance monitoring. The method applicability was checked by analyzing 30 fish samples collected from local markets. Two fish samples surpassed the established MRL of 100 μg kg−1 with values of 104 μg kg−1 and 112 μg kg−1.

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