Improved method for the on-line metal chelate affinity chromatography–high-performance liquid chromatographic determination of tetracycline antibiotics in animal products

Cooper, Andrew; Stubbings, G. W.; Kelly, Mitchell; Tarbin, J. A.; Farrington, William H. H.; Shearer, George

doi:10.1016/s0021-9673(97)01290-9

Cited by 82 publications

(47 citation statements)

References 7 publications

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“…SPME may therefore prove to be a useful screening technique for the identification of tetracycline contamination prior to performing a more sensitive but equally more costly and lengthy analysis by metal chelate affinity chromatography followed by high performance chromatography. 7,15 The Carbowax/templated resin fibre proved the most efficient at extracting the analytes, closely followed by the Carbowax/divinylbenzene fibre. The restricted variety of fibres initially available for the study is an obvious limitation to a more widespread development of the SPME/ LC/MS method.…”

Section: Discussionmentioning

confidence: 98%

“…13 This property has been utilised in the development of metal chelate affinity chromatography (MCAC) as a selective clean-up technique prior to the HPLC analysis of tetracyclines. 5,[14][15][16] However, the eluant from the MCAC still contains components detrimental to the performance of the HPLC column, and C 18 solid phase extraction or ultrafiltration have been described as further de-proteinisation steps. 5 The application of HPLC/MS confers a significant advantage in the confirmation of residual tetracyclines.…”

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confidence: 99%

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Rapid analysis of tetracycline antibiotics by combined solid phase microextraction/high performance liquid chromatography/mass spectrometry

Lock

Chen

Volmer

1999

Rapid Commun. Mass Spectrom.

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The technique of solid phase microextraction (SPME) combined on-line with high performance liquid chromatography/mass spectrometry (HPLC/MS) has been applied to the analysis of seven tetracycline analogues. Rapid baseline separation was achieved in under 5 min using a short 3 microm RP-18e cartridge column. Optimisation of the SPME procedure is described including choice of extracting fibre and modification of the sample by heating or salting out of the analytes. Detection limits of 4-40 ng/mL were obtained for the various analogues from extracted aqueous samples and absolute amounts of analyte extracted by the method determined using external calibration. To demonstrate the applicability of the technique for real samples the extraction of tetracycline from milk is described.

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Section: Discussionmentioning

confidence: 98%

mentioning

confidence: 99%

Rapid analysis of tetracycline antibiotics by combined solid phase microextraction/high performance liquid chromatography/mass spectrometry

Lock

Chen

Volmer

1999

Rapid Commun. Mass Spectrom.

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“…As described above, TCs have a chelating ability, which has been used to establish a clean-up method, such as metal chelate affinity chromatography (12,14). However, this method requires complicated procedures and gives poor recovery and reproducibility.…”

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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“…Walsh et al (21) used a 0.1 M EDTAMcIlvaine buffer that resulted in more consistent recoveries for tetracyclines extracted from meat samples. Metal-chelating affinity chromatography (MCAC) has also been used for the clean-up of tetracyclines in food, serum, and urine samples (6). However, an additional desalting step of eluent from the MCAC column is required prior to analysis by LC-MS. Solid-phase microextraction (SPME) may be problematic for complex biological matrices due to its reduced loading capacity, and may not be convenient for routine analysis (26).…”

Section: Discussionmentioning

confidence: 99%

Screening method for the determination of selected tetracyclines in water by liquid chromatography with diode array detector

Patyra

Kowalczyk

Kwiatek

2014

Bulletin of the Veterinary Institute in Pulawy

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A chromatographic procedure for determination of oxytetracycline (OXT), tetracycline (TC), chlorotetracycline (CTC), and doxycycline (DC) in water samples was developed and was applied for the analysis of water samples collected from poultry and pig farms and environmental water samples. Samples were acidified with trifluoroacetetic acid to pH 3 and further purified by solid phase extraction using Oasis HLB cartridges. The samples were dried up and redissolved in the mixture of oxalic acid and methanol. Separation was performed on reserved phase column (Phenomenex column C 18 , 250 mm × 4.6 mm, 5 µm) by multistep gradient elution, and detection was carried out at 360 nm for OTC and TC, 370 nm for CTC, and 350 nm for DC. The tetracyclines were eluted with the mobile phase of 0.05 M oxalic acid (pH 2.5), acetonitrile, and methanol. This method provided average recoveries of 83.53% to 108.59%, with coefficient of variations (CVs) of 2.41% to 8.64% in the range of 10 to 1000 µg/L OTC, TC, CTC, and DC in water. The linearity for the tetracyclines was determined by HPLC-DAD in the range 10 to 1000 µg/L, with the correlation coefficient (R) > 0.99. The LOD and LOQ for the tetracyclines in water samples ranged from 1.51 to 4.00 and 2.51 to 5.93 µg/L, respectively.

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Improved method for the on-line metal chelate affinity chromatography–high-performance liquid chromatographic determination of tetracycline antibiotics in animal products

Cited by 82 publications

References 7 publications

Rapid analysis of tetracycline antibiotics by combined solid phase microextraction/high performance liquid chromatography/mass spectrometry

Rapid analysis of tetracycline antibiotics by combined solid phase microextraction/high performance liquid chromatography/mass spectrometry

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

Screening method for the determination of selected tetracyclines in water by liquid chromatography with diode array detector

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