Validation methods for the determination of β agonists residues in feed (original) (raw)
Related papers
2018
The use of β-agonists in livestock production is prohibited in many countries because the residues of β-agonists in food pose a potential risk to human health. The present work describes the development and validation of the LC-MS/MS method for detection of ten β-agonists in bovine urine according to Commission Decision 2002/657/EC requirements. Linearity of the method resulted with coefficient of correlation >0.990. The decision limits (CCα) ranged from 0.127 ng/mL to 0.646 ng/mL, and the detection capability (CCβ) resulted in the range 0.140 ng/mL to 0.739 ng/mL. The observed recoveries in the fortified bovine urine samples were satisfactory at every fortification level with values from 73.67% to 118.80%. The coefficient of variation (CV, %) at three fortification levels for each β-agonist was in complete agreement with the requirements from Commission Decision 2002/657/EC. The CV for intraday precision varied from 1.619% to 15.472% and the CV for interday precision varied from...
Meat Science
Forty-eight Bonsmara steers were assigned to three treatment groups and one control group consisting of 12 animals each. The control (C) received no β-agonist, while the three treatment groups received zilpaterol (6 ppm) (Z), ractopamine (30 ppm) (R) or clenbuterol (2 ppm) (Cl) for the last thirty days on feed. Growth performance (final 30 days), USDA quality and yield grades and meat quality (shear force, chemical, histological and biochemical) were compared for the three β-agonist and control groups. Animals responded negatively to Cl treatment during initial stages of supplementation, which was evident in lower feed consumption and initial growth rates. For carcass growth and yield, Cl had greater and more efficient growth rates, higher dressed out yields (proportional), lower USDA yield grades, and reduced marbling compared with C (P < 0.05). For meat quality measurements, the M. longissimus (LL) and M. semitendinosus (ST) were sampled. Cl had the greatest effect (P < 0.05...
Validation of ELISA test kits for detection of beta-agonist residues in meat
The Southeast Asian journal of tropical medicine and public health, 2004
Three ELISA test kits, the Randox ELISA beta-agonist test kit, Euro-Diagnostica test kit, and Ridascreen beta-agonist test kit, were evaluated for screening of meat and liver for beta-agonist residues in fortified and field-incurred samples. It was found that the Randox beta-agonist test kit was more suitable as a screening tool due to its accuracy, ease of use, and lower cost. The tests were able to detect beta-agonist residues at the minimum level of detection, as claimed by the suppliers. The performance of the method as assessed through recovery rates of beta-agonists in fortified samples was satisfactory with a low coefficient of variation (1-3%). Repeatability, as measured through the coefficient of correlation was also satisfactory. For field-incurred positive samples, the test kit showed a sensitivity of 100% and a low rate of false positives for goat and cow tissues. However, a high rate of apparent false positives was obtained for tissues of swine.
Analytica Chimica Acta, 2009
A bioassay was developed for the detection of a broad range of beta-agonist compounds in animal feeds. A solubilised beta2-adrenoceptor was utilised as the binding protein in the assay. This protein was found to be highly stable when stored at 80 degrees C. The assay was developed and initially validated to determine the sensitivity and relative selectivity against a panel of commonly used beta-agonist compounds. It was also shown that when beta-agonists were present as cocktails in samples a pronounced synergistic effect could be measured. The method was further validated according to EC Decision 2002/657 and proved capable of detecting 250ng clenbuterol equivalents per gram of sample. This is well below the quantities normally associated with beta-agonist medicated feeds. The beta2-adrenoceptor used in the study only failed to bind the compound zilpaterol, raising doubts as to whether this compound is a true beta2-adrenergic drug.
Assessment of various veterinary drug residues in animal originated food products
Veterinary World, 2021
The veterinary drugs are broad-spectrum antibacterial antibiotics; it uses to cure the animal disease. Many countries have banned veterinary drug residues like nitrofurans metabolites, chloramphenicol. However, the people were administrated veterinary drugs to animals as illegal to increase the milk production in animals for economic benefit. The results of illegally use of veterinary drugs remain as a residue in animal product like milk and it is very harmful to whom consume it cause cancer and allergic for human being which has entered the concern among milk consumers. To control illegal use of veterinary drugs, the government of India has restricted its use in animals. For the identification and confirmation of veterinary drug residues in animal products, analytical techniques such as liquid chromatography and mass spectrometry are available. These are very sophisticated equipments which are available nowadays and their methodologies for the analytical method validation are described by European commission 2002/657/EC. The use of veterinary drugs is a big challenge to effectively identify and authorization of their use. There are so many analytical techniques are using very effectively and taking very less time to protect the consumers from their adverse effects. These techniques take very less time to identify more groups of compounds such as tetracycline, sulfonamides, anthelmintic, and macrolides in single multi-residue method. These methods having validation parameters include system precision, calibration curve, accuracy, limit of detection, and quantification. Therefore, improvement in the existing technologies and accessibility of new screening methodologies will give opportunities for automation that helps in obtaining the results in very less time and improved sensitivity and specificity which contribute to better safety assurance, standard, and quality of various food products of animal origin.
Food Control, 2015
Because of the risk that residues of antibacterial growth promoters in edible tissues could lead to allergic reactions and development of resistant strains of bacteria in humans, the European Commission decided to ban bacitracin, olaquindox, spiramycin, tylosin and virginiamycin as feed additives. To control the compliance of this ban, a single multi-analyte liquid chromatography-tandem mass spectrometry method was developed in 2003. Starting from this method, we further tried to optimise the response with the aid of experimental design. Using a central composite design, we searched for the optimal extraction solvent for each of the five components separately. As expected, this optimal composition was different for each of these antibacterial growth promoters. Two groups of compounds could be distinguished. The first group contained those compounds (spiramycin, tylosin and virginiamycin) that had the highest response (peak area) when the extraction solvent consisted of pure methanol (with or without the addition of formic acid). The second group contained the components (bacitracin and olaquindox) that preferred between 50 and 70% (v/v) methanol as extraction solvent. To find a compromise between these two groups, we created weighed utility functions and analysed these data with linear regression (α < 0.05). The extraction solvent that gave the overall best response for the type of feed used during this experiment was very similar to the extraction solvent used during the validation of the multi-analyte method (70% (v/v) methanol and 2% (v/v) formic acid) [C.
Rapid Methods for detection of Veterinary Drug residues in Meat
Veterinary World, 2010
The use of substances having hormonal or thyreostatic action as well as b-agonists is banned in many countries. However, sometimes forbidden drugs may be added to feeds for illegal administration to farm animals for promoting increased muscle development or increased water retention and thus obtain an economical benefit. The result is a fraudulent overweight of meat but, what is worse, residues of these substances may remain in meat and may pose a real threat to the consumer either through exposure to the residues, transfer of antibiotic resistance or allergy risk. This has exerted a great concern among the meat consumers. The control of the absence of these forbidden substances in animal foods and feeds is regulated in the European Union by Directive 96/23/EC on measures to monitor certain substances and residues in live animals and animal products. Analytical methodology, including criteria for identification and confirmation, for the monitoring of compliance was also given in Decisions 93/256/EEC and 93/257/EEC. More recently, Decision 2002/657/EC provided rules for the analytical methods to be used in testing of official samples. New substances with anabolic properties are being detected year by year increasing the list of forbidden compounds to be tested. Furthermore, the extended practice consisting in the use of "cocktails" (mixtures of low amounts of several substances that exert a synergistic effect) to have a similar growth promotion, reduces the margin for an effective analytical detection. Thus, the evolution of the "black market" is making really difficult to have an effective analytical control of the residues of these substances in foods of animal origin. Control laboratories must face an increasing demand of analysis like the growing number of residues to be analysed in different types of samples, the strict guidelines for analytical methodologies according to the latest Directives, the increased costs of such new methodologies, the variety of residues to search per sample and the need to invest on powerful new instruments for identification and confirmatory purposes. Rapid and versatile screening methodologies make its control easier and reduce the number of non-compliant samples to be confirmed through tedious and costly confirmatory analytical methodologies. For instance, the multiresidue analysis can be performed better by using fast LC methods. Thus, the availability of new screening methodologies and the improvement of the existing ones will contribute to a better safety assurance of meat and other foods of animal origin.
Bioassay based screening of steroid derivatives in animal feed and supplements
Analytica Chimica Acta, 2011
Receptor binding transcription activation bioassays are valuable tools for the screening of steroid hormones in animal feed and supplements. However, steroid derivatives often lack affinity for their cognate receptor and do not show any direct hormonal activity by themselves. These compounds are thus not detected by these kinds of bioassays and need a bioactivation step in order to become active, both in vivo and in vitro. In this study a comparison was made between different in vitro activation methods for hormone esters and hormone glycosides. Testosterone acetate and testosterone decanoate were chosen as model compounds for the hormone esters, representing the broad range of steroid esters of varying polarities, while genistin was used as a substitute model for the steroid-glycosides. Concerning bioactivation of the steroids esters, the efficiency for alkaline hydrolysis was 90-100% and much better as compared to enzymatic deconjugation by esterase. As a result 1 g testosterone ester per gram of animal feed could easily be detected by a yeast androgen bioassay. When comparing different enzyme fractions for deglycosilation, genistin was shown to be deconjugated most efficiently by -glucuronidase/aryl sulfatase from Helix pomatia, resulting in a significant increase of estrogenic activity as determined by a yeast estrogen bioassay. In conclusion, chemical and enzymatic deconjugation procedures for ester and glycoside conjugates respectively, resulted in a significant increase in hormonal activity as shown by the bioassay readouts and allowed effective screening of these derivatives in animal feed and feed supplements.
Recent Advances in the Determination of Veterinary Drug Residues in Food
Foods
The presence of drug residues in food products has become a growing concern because of the adverse health risks and regulatory implications. Drug residues in food refer to the presence of pharmaceutical compounds or their metabolites in products such as meat, fish, eggs, poultry and ready-to-eat foods, which are intended for human consumption. These residues can come from the use of drugs in the field of veterinary medicine, such as antibiotics, antiparasitic agents, growth promoters and other veterinary drugs given to livestock and aquaculture with the aim of providing them as prophylaxis, therapy and for promoting growth. Various analytical techniques are used for this purpose to control the maximum residue limit. Compliance with the maximum residue limit is very important for food manufacturers according to the Food and Drug Administration (FDA) or European Union (EU) regulations. Effective monitoring and control of drug residues in food requires continuous advances in analytical...
Methods for Screening Veterinary Drug Residues in Animal Products: A review
2016
يرطيبلا ة لأا يناويحلا تاجتنملا ىف ىرخ ة . Summary With strict regulations and government controls worldwide, the monitoring of animal drug residues is becoming increasingly complex and demanding. The risk of failing to comply with legally permitted maximum limits can affect consumer health. For this reason, accurate results of residue levels in animal products are needed. International food safety authorities outline the concept of reference method criteria in which minimum requirements of analytical methods used in the analysis of veterinary drug residues, being screening or confirmatory, were described. In this document, the most important analytical methods used in the screening of antimicrobial and some other veterinary drug residues were described.