Validation Study for the Determination of Tetracycline Residues in Animal Tissues (original) (raw)
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Molecules
We examined a total of 369 bovine liver and muscle samples for the detection of oxytetracycline (OTC), tetracycline (TC), chlortetracycline (CTC), and doxycycline (DOX) residues by implementation and validation of a LC-MS/MS method. The method showed good recovery values between 86% and 92% at three levels of concentrations. The linearity tests revealed r2 > 0.996 for all the tetracyclines examined. Furthermore, the Youden test revealed that the method was robust. Only 14.4% of the samples showed OTC and TC residues in a concentration range of 10.4–40.2 µg kg−1. No CTC and DOX residues were found in all the samples analyzed. Liver samples showed the highest average values (31.5 ± 20.6 and 21.8 ± 18.9 for OTC and TC, respectively). The results showed a low incidence of TCs in all the samples examined, in comparison with other studies reported in the literature. A significant decrease in TC residues frequency was found from 2013 (p < 0.05). This work reports for the first time e...
Iranian Journal of Pharmaceutical Research (2012), 11 (3): 781-787
Edible cattle tissues from local markets of Ardabil, Iran were examined for residues of tetracycline antibiotics (tetracycline, oxytetracycline and chlortetracycline). In total, 110 samples of triceps, gluteal muscle, diaphragm, kidney and liver were randomly obtained from the local markets of the city of Ardabil. Solid-phase extraction (SPE) and highperformance liquid chromatography (HPLC) methods were used to extract and analyze tetracycline antibiotics (TC) residues, respectively. The mean amount of total TC residues in all samples tested was 226.3 ± 112.5 ng/g; the mean amount of the total TC residues in triceps, gluteal muscle, diaphragm, kidney and liver samples were 176.3 ± 46.8, 405.3 ± 219.6, 96.8 ± 26.9, 672.4 ± 192.0 and 651.3 ± 210.1 ng/g, respectively. Additionally, 25.8% of muscle samples, 31.8% of liver samples and 22.7% of kidney samples contained amounts of TC residues beyond the maximum residue limit (MRLs). To reduce the TC residues found in edible cattle tissues, regulatory authorities should ensure that cattle undergo the proper withdrawal period from TCs before slaughtering. Keywords: Tetracycline; Meat; Liver; Kidney; HPLC.
The Analyst, 1998
An interlaboratory study was organised in 1996 in order to determine laboratory testing performance for measuring oxytetracycline (OTC) and 4-epioxytetracycline (4-epiOTC) residues in pig muscle. The organisation was designed according to the 'International Harmonised Protocol for Proficiency Testing of (Chemical) Analytical Laboratories' produced by the Association of Official Analytical Chemists (AOAC International) and the International Union of Pure and Applied Chemistry (IUPAC). Fourteen National Reference Laboratories (NRLs) out of the 15 asked to participate agreed to analyse the samples. These laboratories were from 13 different European Union (EU) Member States and each participant was allowed to use the extraction method of their own choice but had to use liquid chromatography as the analytical technique. Most of the methods used were based on UV detection (simple wavelength or diode-array detection) but some involved fluorimetric detection. The production of incurred samples was prepared on-site. The OTC and 4-epiOTC concentrations present in the samples were determined by taking the mean of the results (excluding outliers) and the deviation of each result from the assigned value was measured. The performance of the laboratories was evaluated by calculating the 'z-scores'. The results were globally satisfactory and showed that all 14 laboratories were capable of determining OTC and 4-epiOTC in pig muscle with satisfactory accuracy. Only two laboratories obtained a questionable result in terms of repeatability.
A new bioassay method for quantitative analysis of tetracyclines
2004
A new method is described for quantitative analysis of tetracycline, based on the decrease in external pH of bacterial suspensions after the addition of a glucose pulse. The decrease in external pH of these suspensions was inversely proportional to the concentration of tetracycline. The correlation coefficient of standard response lines derived from the bioassay was 0.99. Tetracycline potency was determined in six tetracycline HCl samples by the sugar pulse bioassay and a turbidimetric method. The turbidimetric assay result varied from the glucose-pulse data by no more than 7 and 3% at 3 and 7 min, respectively. The procedure is rapid, precise and quantitative, and requires minimal preparation and use of media, with savings in laboratory resources and time.
2019
Tetracycline antibiotics (TCs) have been widely employed to treat bacterial infections and other pathologic conditions in humans and pets. Although most of TCs have been almost ruled out from the human clinical practice they are still used as growth promoters and to treat promiscuity and overcrowding pathologies in the intensive animal farming. As a consequence, TCs are commonly found in all ecological compartments with potential direct or indirect toxicological effects on animals and, generally, on all living organisms. Moreover, clinical and in vitro observations raised the hypothesis that the widespread of some adverse food reactions and, to a less extent, antibiotic resistance phenomena could be ascribed to the presence of TCs residues in edible and non-edible tissues of intensive animal farming intended for animal and human consumption. Such residues may pose serious health threat, depending on the type of food and the amount of residue present. The aim of this review is to provide new insights about the clinical uses of TCs in humans and animals and their potential toxic effects as residues in the environment or as food components.
Egyptian Journal of Animal Health
A ntibiotics are extensively used in animal husbandry practices for the treatment of diseases. Four tetracyclines are commercially available as veterinary medicines, of which oxytetracycline (OTC), tetracycline (TC), chlortetracycline (CTC), and doxycycline (DOX). In the present investigation, a novel simple, sensitive, and inexpensive method of analysis was verified for tetracyclines by RP-HPLC system in bulk drug substance and pharmaceutical forms via two stationary phases (C8 & C18). The separation was attained on a 250 mm column length, 4.6 mm internal diameter, 5 µm particle size, C18 and C8 columns with a (55:25:20) 5% glacial acetic acid: acetonitrile: methanolic acid as elution solution at a 355 nm wavelength. The method was performed at a0.8 ml/m inflow rate. This method was applied without an extraction process. The method was validated following ICH and USP guidelines. It was proved to be reproducible and more economical due to the short retention time of less than 6 min by C8 column and 8 min by C18 column which enabled analysis of tetracycline pharmaceutical products with a relatively lower volume of mobile phase. The result of formulation analysis was statistically validated with a high recovery percentage. Furthermore, the developed method was free from the interference of excipients used in the formulation. The validated method was accurate, precise, linear, and reproducible. The data suggest the possibility of using the method in quality control laboratories with better routine analysis of tetracyclines in their dosage forms.
Journal of Agricultural and Food Chemistry, 2007
A sensitive and specific method is described for the simultaneous determination of oxytetracycline, tetracycline (TC), and chlortetracycline residues in edible swine tissues, by combining liquid chromatography with spectrofluorometric and mass spectrometry detection. The procedure involved a preliminary extraction with EDTA-McIlvaine buffer acidified at pH 4.0, followed by solid-phase extraction cleanup using a polymeric sorbent. The liquid chromatography analysis was performed with spectrofluorometric detection after postcolumn derivatization with magnesium ions. The limits of quantification were 50 µg/kg for muscle and 100 µg/kg for kidney tissues. The recovery values were greater than 77.8% for muscle and 65.1% for kidney. The method has been successfully used for the quantification of tetracyclines in swine tissues samples. The selective liquid chromatography mass spectrometric analysis for confirmation of oxytetracycline in one positive swine muscle sample was made by atmospheric pressure chemical ionization (APCI). The APCI mass spectra of the TCs gave the protonated molecular ion and two typical fragment ions, required for their confirmation in single ion monitoring scan mode in animal tissues.
Journal of AOAC International
A fast, sensitive, and specific liquid chromatographic/tandem mass spectrometric method was developed and validated for determination of tetracycline in human plasma. Tetracycline and oxytetracycline [internal standard (IS)] were extracted from the plasma by protein precipitation. The mobile phase consisted of acetonitrile-formic acid 0.1% (48 + 52, v/v), run at a flow rate of 1 ml/min (split 1:5). Detection was performed by positive electrospray ionization in multiple reaction monitoring mode, monitoring the transitions 444.8 > 410.0 and 461.0 > 426.0 for tetracycline and IS, respectively. The analysis was performed in 3.5 min and the method was linear in the plasma concentration range of 50-6000 ng/mL. The mean extraction recoveries for tetracycline and IS from plasma were 92.14 and 94.04%, respectively. Method validation investigated parameters such as the linearity, precision, accuracy, specificity, and stability, giving results within the acceptable range. The proposed me...