Development of a High Pressure Liquid Chromatography with Diode Array Detection Method for the Determination of Four Tetracycline Residues in Milk by Using QuEChERS Dispersive Extraction
QuEChERS (quick, easy, cheap, effective, rugged and safe) dispersive extraction was applied for the extraction of tetracyclines (oxytetracycline, tetracycline, chlorotetracycline and doxycycline) from milk. Target analytes were determined by an accurate and sensitive chromatographic analytical metho...
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MDPI AG
2019-04-01
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Online Access: | https://www.mdpi.com/2297-8739/6/2/21 |
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author | Eirini Marinou Victoria F. Samanidou Ioannis N. Papadoyannis |
author_facet | Eirini Marinou Victoria F. Samanidou Ioannis N. Papadoyannis |
author_sort | Eirini Marinou |
collection | DOAJ |
description | QuEChERS (quick, easy, cheap, effective, rugged and safe) dispersive extraction was applied for the extraction of tetracyclines (oxytetracycline, tetracycline, chlorotetracycline and doxycycline) from milk. Target analytes were determined by an accurate and sensitive chromatographic analytical method, which was validated in terms of 2002/6572/EC decision. The analytes were separated on an Orbit 100C<sub>4</sub> (5 μm, 250 × 4.0 mm) analytical column under a gradient mobile phase composed of a mixture of 0.01 M oxalic acid, 10<sup>−4</sup> M Na<sub>2</sub>EDTA and acetonitrile. For the extraction of isolated compounds from sorbent, a methanol and 0.01 M oxalic acid mixture (1:1 <i>v</i>/<i>v</i>) was used, leading to relative recovery rates from 83.07% to 106.3% at concentration levels in the range 100–200 μg/kg. The within-laboratory reproducibility, expressed as a relative standard deviation, was <15.5%. Decision limits ranged between 100.3 μg/kg and 105.6 μg/kg and the detection capability varied between 100.6 μg/kg and 109.7 μg/kg. Ruggedness was evaluated by following the Youden approach, in terms of milk mass, sorbent mass, centrifugation time, vortex time, type and volume of organic solvents and evaporation temperature. |
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issn | 2297-8739 |
language | English |
last_indexed | 2024-04-13T06:51:51Z |
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spelling | doaj.art-f310667041b548e9beb450daf1bfa6ac2022-12-22T02:57:23ZengMDPI AGSeparations2297-87392019-04-01622110.3390/separations6020021separations6020021Development of a High Pressure Liquid Chromatography with Diode Array Detection Method for the Determination of Four Tetracycline Residues in Milk by Using QuEChERS Dispersive ExtractionEirini Marinou0Victoria F. Samanidou1Ioannis N. Papadoyannis2Laboratory of Analytical Chemistry, Department of Chemistry, School of Sciences, Aristotle University of Thessaloniki, Thessaloniki 54124 GR, GreeceLaboratory of Analytical Chemistry, Department of Chemistry, School of Sciences, Aristotle University of Thessaloniki, Thessaloniki 54124 GR, GreeceLaboratory of Analytical Chemistry, Department of Chemistry, School of Sciences, Aristotle University of Thessaloniki, Thessaloniki 54124 GR, GreeceQuEChERS (quick, easy, cheap, effective, rugged and safe) dispersive extraction was applied for the extraction of tetracyclines (oxytetracycline, tetracycline, chlorotetracycline and doxycycline) from milk. Target analytes were determined by an accurate and sensitive chromatographic analytical method, which was validated in terms of 2002/6572/EC decision. The analytes were separated on an Orbit 100C<sub>4</sub> (5 μm, 250 × 4.0 mm) analytical column under a gradient mobile phase composed of a mixture of 0.01 M oxalic acid, 10<sup>−4</sup> M Na<sub>2</sub>EDTA and acetonitrile. For the extraction of isolated compounds from sorbent, a methanol and 0.01 M oxalic acid mixture (1:1 <i>v</i>/<i>v</i>) was used, leading to relative recovery rates from 83.07% to 106.3% at concentration levels in the range 100–200 μg/kg. The within-laboratory reproducibility, expressed as a relative standard deviation, was <15.5%. Decision limits ranged between 100.3 μg/kg and 105.6 μg/kg and the detection capability varied between 100.6 μg/kg and 109.7 μg/kg. Ruggedness was evaluated by following the Youden approach, in terms of milk mass, sorbent mass, centrifugation time, vortex time, type and volume of organic solvents and evaporation temperature.https://www.mdpi.com/2297-8739/6/2/21HPLCmilkQuEChERStetracyclines |
spellingShingle | Eirini Marinou Victoria F. Samanidou Ioannis N. Papadoyannis Development of a High Pressure Liquid Chromatography with Diode Array Detection Method for the Determination of Four Tetracycline Residues in Milk by Using QuEChERS Dispersive Extraction Separations HPLC milk QuEChERS tetracyclines |
title | Development of a High Pressure Liquid Chromatography with Diode Array Detection Method for the Determination of Four Tetracycline Residues in Milk by Using QuEChERS Dispersive Extraction |
title_full | Development of a High Pressure Liquid Chromatography with Diode Array Detection Method for the Determination of Four Tetracycline Residues in Milk by Using QuEChERS Dispersive Extraction |
title_fullStr | Development of a High Pressure Liquid Chromatography with Diode Array Detection Method for the Determination of Four Tetracycline Residues in Milk by Using QuEChERS Dispersive Extraction |
title_full_unstemmed | Development of a High Pressure Liquid Chromatography with Diode Array Detection Method for the Determination of Four Tetracycline Residues in Milk by Using QuEChERS Dispersive Extraction |
title_short | Development of a High Pressure Liquid Chromatography with Diode Array Detection Method for the Determination of Four Tetracycline Residues in Milk by Using QuEChERS Dispersive Extraction |
title_sort | development of a high pressure liquid chromatography with diode array detection method for the determination of four tetracycline residues in milk by using quechers dispersive extraction |
topic | HPLC milk QuEChERS tetracyclines |
url | https://www.mdpi.com/2297-8739/6/2/21 |
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