Validation of a high-performance liquid chromatography method for the determination of oxytetracycline, tetracycline, chlortetracycline and doxycycline in bovine milk and muscle

Cinquina, A. L.; Longo, Francesca; Anastasi, G.; Giannetti, Luigi; Cozzani, R.

doi:10.1016/s0021-9673(02)01446-2

Cited by 286 publications

(162 citation statements)

References 7 publications

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“…Since TCs have good water solubility, solid phase extraction is the preferred method for their extraction. For the clean-up purposes several types of SPE cartridges were presented in the literature: C18 (30), polymeric (9,28), carboxylic acid (17,18), styrene-divinylbenzene (29), or cyklohexyl (22). 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.…”

Section: Discussionmentioning

confidence: 99%

“…Using a mass spectrometer for antibacterial compound detection offers many advantages, such as independence from a chromophor and fluorophor, the possibility of structural information, lower detection limits, and easier separation of co-eluting peaks (26). Although the degradation products of TCs and the presence of epimers of OTC, TC, and CTC was proven, there are still many HPLC-based methods suitable for determination of parent compounds only (3,9,25,28,31). For screening purposes, the determination of TCs with their degradation products does not require additional confirmatory methods, usually based on liquid chromatography -tandem mass spectrometry (LC-MS/MS); however, the quantitative analysis of TCs should also include TC epimers.…”

Section: Introductionmentioning

confidence: 99%

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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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Section: Discussionmentioning

confidence: 99%

Section: Introductionmentioning

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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“…Recovery values were considered satisfactory for chicken-muscle samples in all fortification levels and were in the range of 89.38 and 106.27%, similar to obtained from other matrices such as bovine, swine, shrimp, fish and milk. 1,[32][33][34] A relative standard deviation (RSD) up to 20% for within-day precision is acceptable according to European Union decision and Codex Alimentarius. Table 4 presents the within-day precision of the method at the 3 different levels of interest; these were considered satisfactory for all TCs.…”

Section: Accuracy and Precision (Within-day And Between-day)mentioning

confidence: 99%

“…The values for CCα and CCβ were in accordance to other studies of TCs in other food matrices. 21,24,34 …”

Section: Decision Limit (Ccα) and Detection Capability (Ccβ)mentioning

confidence: 99%

Development and validation of a method for the analysis of tetracyclines in chicken-muscle by liquid chromatography-electrospray-mass spectrometry in tandem (LC-ESI-MS/MS)

Uekane¹,

Neto²,

Gomes³

2011

Quím. Nova

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Recebido em 20/12/09; aceito em 8/7/10; publicado na web em 9/11/10 A LC-ESI-MS/MS method was developed and validated according to the European Union decision 2002/657/EC, for the determination of tetracyclines (TCs) in chicken-muscle since Europe is one of the main markets for Brazilian products. Linearity of r > 0.9979, limits of quantification in the range of 7.0-35.0 ng/g, average recoveries of 89.38 -106.27%, within-day and betweenday precision were adequate for all TCs. The decision limit and the detection capability were 93.00-106.46 ng/g and 95.84-114.38 ng/g, respectively. This method is suitable for application in surveillance programmes of residues of TCs in chicken-muscle samples.

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“…The major worldwide public concern and health hazard associated with antibiotic residues in animal products is the development of resistant bacterial strains of animal origin and its consequent effect on human health (Aarestrup, 2005). To ensure human food safety, worldwide regulatory authorities such as World Health Organization (1999), and Food and Agriculture Organization (2008), have set maximum residue limits (MRLs) for several veterinary drugs in foods, as well as acceptable daily intake (ADI) of antibiotics by humans (Cinquina et al, 2003;Fritz and Zuo, 2007).…”

Section: Introductionmentioning

confidence: 99%

Assessment of microbiological and residual antibiotics status in milk sold in Abeokuta, Ogun State. Nigeria

Oluwafemi

Oluwabamiwo

Oluwatosin

et al. 2018

Turkish JAF Sci.Tech.

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This study investigated the prevalence and concentration of antibiotic residues in twenty brands of milk. Determination and quantification of antibiotic residues was done using High Performance Liquid Chromatography. Aerobic plate count was carried out and the associated bacteria isolated. Identification of bacteria was done using standard microbiological methods. Molecular characterization and identification of bacterial isolates was done using 16S rRNA gene sequencing method. Antibiotic sensitivity was carried out on bacterial isolates using disc diffusion method. Plasmid profile of drug resistant isolates was done using alkaline analysis method. Comparison of means was done using Analysis of Variance. Antibiotic residues were detected in 10 (50%) of the 20 milk brands analyzed. The residual levels of tetracycline, oxytetracycline and chlortetracycline ranged between 5ng/kg and 1569ng/kg while none of the samples had doxycycline residues. The prevalence of tetracycline residues in evaporated milk brands and powdered milk samples were 100 and 23 % respectively. The aerobic plate counts ranged from 2.5 × 10 2 to 6.5 × 10 2 CFU∕mL for evaporated milk and 2.5 × 10 1 to 6.0 × 10 1 CFU∕mL for powdered milk. A total of ten bacterial species were isolated and identified. Susceptibility result showed that 95% of the isolates were sensitive to erythromycin, cefuroxime and gentamycin; 12.5% were resistant to tetracycline and ampicillin, 10% were resistant to ofloxacin and 7.5% to doxycycline and penicillin. Five of the bacterial isolates were resistant to more than one class of antibiotics. Resistant isolates subjected to plasmid profiling had detectable plasmids with estimated sizes between 120bp and 1000bp. The obtained results provide evidence that the presence of antibiotic residues in evaporated and powdered milk is an indication that the public is exposed to the harmful effects of the residues.

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Validation of a high-performance liquid chromatography method for the determination of oxytetracycline, tetracycline, chlortetracycline and doxycycline in bovine milk and muscle

Cited by 286 publications

References 7 publications

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

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

Development and validation of a method for the analysis of tetracyclines in chicken-muscle by liquid chromatography-electrospray-mass spectrometry in tandem (LC-ESI-MS/MS)

Assessment of microbiological and residual antibiotics status in milk sold in Abeokuta, Ogun State. Nigeria

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