Complexities in tetracycline analysis—chemistry, matrix extraction, cleanup, and liquid chromatography

Anderson, Collin; Rupp, Heidi S; Wu, Wen‐Hsin

doi:10.1016/j.chroma.2005.04.013

Cited by 211 publications

(104 citation statements)

References 63 publications

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“…As regard tetracyclines, they have the highest capability to bind organic matter [6] if compared to other antimicrobials, and thus they usually locate in the top layer of soil, within the first 40 cm depth.…”

Section: Introductionmentioning

confidence: 99%

Oxytetracycline as environmental contaminant in arable lands

Brambilla

Patrizii

Filippis

et al. 2007

Analytica Chimica Acta

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Oxytetracycline (OXY) is a broad-range antimicrobial routinely used in pig production, at doses in the range of few g/kg of medicated feed, during the weaning period. It could persist at ppm level in pig liquid manure that routinely is used for organic fertilisation. In the present work we describe a methodology to study OXY environmental fate in arable land where crops are cultivated for animal feeding purposes. A liquid-liquid extraction followed by metal chelate affinity chromatography was applied to environmental samples of manures and soils drawn within a case-control study. Extracts were then analysed by high performance liquid chromatography with UV/DAD detection, using a reverse phase column, and expressing the results as 4-epioxytetracycline epimer. Results indicate OXY is well retained at mg kg −1 levels in soil exposed to contaminated pig manure fertilisation. Such compartment could constitute an abiotic reservoir for the systemic and/or for the external contamination of corn.

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Section: Introductionmentioning

confidence: 99%

Oxytetracycline as environmental contaminant in arable lands

Brambilla

Patrizii

Filippis

et al. 2007

Analytica Chimica Acta

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“…Tetracyclines typically provided a lower recovery, which is expected due to the typical use of McIlvaine/ EDTA buffer for extraction. [14] It is considered a benefit for screening and identification purposes that the tetracyclines be included and consistent recoveries and reproducibilities makes quantification possible depending on acceptability criteria. Similarly, selected anthelminthics, tranquilizers/NSAIDS, and 'other' vet drugs displayed lower recoveries, but often with higher variability, making quantification unreliable.…”

Section: Quantificationmentioning

confidence: 99%

Evaluation of a multi‐class, multi‐residue liquid chromatography – tandem mass spectrometry method for analysis of 120 veterinary drugs in bovine kidney

Schneider

Lehotay

Lightfield

2012

Drug Testing and Analysis

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Traditionally, regulatory monitoring of veterinary drug residues in food animal tissues involves the use of several single-class methods to cover a wide analytical scope. Multi-class, multi-residue methods (MMMs) of analysis tend to provide greater overall laboratory efficiency than the use of multiple methods, and liquid chromatography-tandem mass spectrometry (LC-MS/MS) of targeted drug analytes usually provides exceptional performance even for complicated sample extracts. In this work, an LC-MS/ MS method was optimized and validated in a test of 120 drug analytes from 11 different classes in bovine kidney. The method used 10 ml of 4/1 acetonitrile/water for extraction of 2 g samples and cleanup with hexane partitioning. Quantitative and qualitative performance was assessed for the analytes at fortification levels of 10, 50, 100, and 200 ng/g. With the method, 66 drugs gave 70-120% recovery with ≤20% RSD at all levels over the course of 3 days. At the 200 ng/g level, 89 drugs met these same standards. Limits of detection were ≤10 ng/g for 109 of the analytes in the kidney matrix in validation experiments. Qualitatively, MS/MS identification criteria were set that ion ratios occur within AE10% (absolute value) from those of the analyte reference standards. At the 10 ng/g level, 57% of the drugs met the identification criteria, which improved to 84% at the 200 ng/g level. The method serves as an efficient and useful additional option among the current monitoring methods available. Published 2012. This article is a U.S. Government work and is in the public domain of the USA.

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“…However, after our comparison of different SPE packings, the polymeric Strata X was found the most efficient because of the highest recovery and cleanest extract and this kind of sorbent was finally selected. It was found that because the columns are made of polymer there were no Ca 2+ residues and no silanol effect (1).…”

Section: Discussionmentioning

confidence: 99%

“…Additionally, TCs are strongly sensitive to light exposure and acidic conditions (1). For effective extraction of TCs from tissues with high extraction efficiency, buffers within the range of 4.0 -5.0 pH values are recommended (20).…”

Section: Discussionmentioning

confidence: 99%

Liquid chromatography – tandem mass spectrometry method for the determination of ten tetracycline residues in muscle samples

Gajda

Posyniak

2015

Bulletin of the Veterinary Institute in Pulawy

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A liquid chromatography -tandem mass spectrometry (LC-MS/MS) method for the determination of oxytetracycline (OTC), 4-epi oxytetracycline (4-epi OTC), tetracycline (TC), 4-epi tetracycline (4-epi TC), chlortetracycline (CTC), 4-epi chlortetracycline (4-epi CTC), doxycycline (DC), minocycline (MINO), methacycline (META) and rolitetracycline (ROLI) residues in muscles was developed. The procedure consisted of an oxalic acid extraction followed by protein removal with trichloroacetic acid. Further solid phase clean-up on polymeric (Strata X) reversed phase columns was performed to obtain an extract suitable for LC-MS/MS analysis. The tetracyclines were separated on a C 18 analytical column with mobile phase consisting of 0.01% formic acid in acetonitrile and 0.01% formic acid in water in gradient mode. The method was validated according to the Commission Decision 2002/657/EC. The recoveries of all target compounds were 91.8% -103.6%. The decision limits were from 109.0 to 119.8 µg/kg and detection capability varied within the range of 122.2 to 137.6 µg/kg, depending on the analyte.

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Complexities in tetracycline analysis—chemistry, matrix extraction, cleanup, and liquid chromatography

Cited by 211 publications

References 63 publications

Oxytetracycline as environmental contaminant in arable lands

Oxytetracycline as environmental contaminant in arable lands

Evaluation of a multi‐class, multi‐residue liquid chromatography – tandem mass spectrometry method for analysis of 120 veterinary drugs in bovine kidney

Liquid chromatography – tandem mass spectrometry method for the determination of ten tetracycline residues in muscle samples

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