Development of analytical methods for multiresidue determination of quinolones in pig muscle samples by liquid chromatography with ultraviolet detection, liquid chromatography–mass spectrometry and liquid chromagraphy–tandem mass spectrometry

2006 ◽  
Vol 1104 (1-2) ◽  
pp. 132-139 ◽  
Author(s):  
M.P. Hermo ◽  
D. Barrón ◽  
J. Barbosa
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Analytical Methods ◽  
Tandem Mass ◽  
Liquid Chromatography Mass Spectrometry ◽  
Ultraviolet Detection ◽  
Pig Muscle ◽  
Multiresidue Determination

scholarly journals Multiresidue Determination of Quinolone and Fluoroquinolone Antibiotics in Fish and Shrimp by Liquid Chromatography/Tandem Mass Spectrometry

2007 ◽  
Vol 90 (2) ◽  
pp. 604-612 ◽  
Author(s):  
Guy Dufresne ◽  
Andre Fouquet ◽  
Don Forsyth ◽  
Sheryl A Tittlemier
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Solid Phase ◽  
Tandem Mass ◽  
Fluoroquinolone Antibiotics ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Multiresidue Determination

Abstract A multiresidue method was developed to measure low levels of 8 fluoroquinolones (norfloxacin, ofloxacin, danofloxacin, ciprofloxacin, desethylene ciprofloxacin, enrofloxacin, sarafloxacin, and difloxacin) and 4 quinolones (oxolinic acid, flumequine, nalidixic acid, and piromidic acid). Method detection limits range from 0.1 ng/g for quinolones to 0.4 ng/g for fluoroquinolones. Average recoveries range from 57 to 96%, depending on analyte and commodity; relative standard deviations are all less than 18%. The drugs are extracted from tissues using a mixture of ethanol and 1% acetic acid, diluted in aqueous HCl, and defatted by extraction with hexane. The compounds are further isolated using cation-exchange solid-phase extraction and measured using liquid chromatography with electrospray tandem mass spectrometry detection. The method has been evaluated and applied to the analysis of salmon, trout, and shrimp. Detectable residues were observed in 10 out of 73 samples, at concentrations ranging from 0.28 to 16 ng/g.

scholarly journals Determination of Chlormequat and Mepiquat in Foods by Liquid Chromatography/Mass Spectrometry or Liquid Chromatography/Tandem Mass Spectrometry: Interlaboratory Study

2005 ◽  
Vol 88 (6) ◽  
pp. 1762-1776 ◽  
Author(s):  
Lutz Alder ◽  
James R Startin ◽  
S Alonso ◽  
T Anspach ◽  
S Brewin ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Wheat Flour ◽  
Good Method ◽  
Tandem Mass ◽  
Liquid Chromatography Mass Spectrometry ◽  
Method Performance ◽  
Fruit Purée

Abstract Interlaboratory validation studies have been performed on 2 methods for the determination of chlormequat (CLQ) and mepiquat (MPQ). Both methods used identical extraction procedures and stable isotope internal standardization but differed in the use of liquid chromatography/mass spectrometry (LC/MS) or LC/tandem mass spectrometry (LC/MS/MS) for the determination, the amount of internal standard used, and the expected limit of detection. After addition of deuterated internal standards, CLQ and MPQ were extracted with methanol–water and determined by LC/MS or LC/MS/MS with positive electrospray ionization. Eight European laboratories participated in the LC/MS method study, analyzing mushroom, pear, wheat flour, and fruit puree with residues of CLQ in the range 0.040–1.19 mg/kg and of MPQ in the range 0.041–0.39 mg/kg. For CLQ, the Horwitz ratio (HoRat) values for individual test materials/levels were in the range 0.85–1.13 with amean of 1.00, showing good method performance. For MPQ, the Ho values for mushroom, pear (both levels), and wheat flour were in the range 0.83–0.94, again indicating good method performance. For the determination of MPQ in infant food (fruit puree) at 0.041 mg/kg, the Ho was 1.7 when a value of 0 reported by one participant was excluded. In the LC/MS/MS study, in which 11 laboratories participated, a separate sample set was analyzed with residues of CLQ in the range 0.007–1.03 mg/kg and of MPQ in the range 0.008–0.72 mg/kg. Ho values for CLQ were in the range 0.27–1.36 and for MPQ in the range 0.51–2.10, all corresponding to acceptable method performance.

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