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Merck

Multidetection of antibiotics in liver tissue by ultra-high-pressure-liquid-chromatography-tandem mass spectrometry.

Journal of chromatography. B, Analytical technologies in the biomedical and life sciences (2014-12-08)
Andreia Freitas, Jorge Barbosa, Fernando Ramos
ABSTRAKT

A multiresidue quantitative screening method covering 39 antibiotics from 7 different families by ultra-high-pressure-liquid-chromatography-tandem mass spectrometry (UHPLC-MS/MS) is described. Sulfonamides, trimethoprim, tetracyclines, macrolides, quinolones, penicillins and chloramphenicol are simultaneously detected in liver tissue. A simple sample treatment method consisting of extraction with a mixture of acetonitrile and ethylenediaminetetraacetic acid (EDTA) followed by solid-phase extraction (SPE) with a hydrophilic-lipophilic balanced (HLB) cartridge was developed. The methodology was validated, in accordance with Decision 2002/657/EC, by evaluating the following required parameters: decision limit (CCα), detection capability (CCβ), specificity, repeatability and reproducibility. The precision, in terms of the relative standard deviation, was under 22% for all of the compounds, and the recoveries were between 80% and 110%. The CCα and CCβ were determined according to the maximum residue limit (MRL) or the minimum required performance limit (MRPL), when established.

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Methanol, suitable for HPLC, gradient grade, suitable as ACS-grade LC reagent, ≥99.9%
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Trimethoprim, ≥98.5%
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Methanol, analytical standard
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Methanol, Absolute - Acetone free
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Acetonitrile(Neat), Pharmaceutical Secondary Standard; Certified Reference Material
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Trimethoprim, United States Pharmacopeia (USP) Reference Standard
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Residual Solvent - Acetonitrile(solution in DMSO), Pharmaceutical Secondary Standard; Certified Reference Material
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Methanol, ACS reagent, ≥99.8%
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Methanol, ACS reagent, ≥99.8%
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Methanol, ACS spectrophotometric grade, ≥99.9%
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