Premium
Determination of metoserpate, buquinolate, and diclofenac in pork, eggs, and milk using liquid chromatography–tandem mass spectrometry
Author(s) -
Park JinA,
Abd ElAty A. M.,
Zheng Weijia,
Kim SeongKwan,
Choi Jeongmin,
Hacımüftüoğlu Ahmet,
Shim JaeHan,
Shin HoChul
Publication year - 2018
Publication title -
biomedical chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 65
eISSN - 1099-0801
pISSN - 0269-3879
DOI - 10.1002/bmc.4215
Subject(s) - chemistry , chromatography , formic acid , detection limit , analyte , tandem mass spectrometry , residue (chemistry) , liquid chromatography–mass spectrometry , mass spectrometry , acetic acid , hexane , calibration curve , biochemistry
In this work, a method was developed for the simultaneous determination of residual metoserpate, buquinolate and diclofenac in pork, milk, and eggs. Samples were extracted with 0.1% formic acid in acetonitrile, defatted with n ‐hexane, and filtered prior to analysis using liquid chromatography–tandem mass spectrometry. The analytes were separated on a C 18 column using 0.1% acetic acid and methanol as the mobile phase. The matrix‐matched calibration curves showed good linearity over a concentration range of 5–50 ng/g with coefficients of determination ( R 2 ) ≥0.991. The intra‐ and inter‐day accuracies (expressed as recovery percentage values) calculated using three spiking levels (5, 10, and 20 μg/kg) were 80–108.65 and 74.06–107.15%, respectively, and the precisions (expressed as relative standard deviation) were 2.86–13.67 and 0.05–11.74%, respectively, for the tested drugs determined in various matrices. The limits of quantification (1 and 2 μg/kg) were below the uniform residual level (0.01 mg/kg) set for compounds that have no specific maximum residue limit (MRL). The developed method was tested using market samples and none of the target analytes was detected in any of the samples. The validated method proved to be practicable for detection of the tested analytes in pork, milk, and eggs.