Determination of aminoglycoside residues in milk and muscle based on a simple and fast extraction procedure followed by liquid chromatography coupled to tandem mass spectrometry and time of flight mass spectrometry

Abstract

Antibiotics are widely used in veterinary medicine mainly for treatment and prevention of diseases. The aminoglycosides are one of the antibiotics classes that have been extensively employed in animal husbandry for the treatment of bacterial infections, but also as growth promotion. The European Union has issued strict Maximum Residue Levels (MRLs) for aminoglycosides in several animal origin products including bovine milk, bovine, swine and poultry muscle. This paper describes a fast and simple analytical method for the determination of ten aminoglycosides (spectinomycin, tobramycin, gentamicin, kanamycin, hygromycin, apramycin, streptomycin, dihydrostreptomycin, amikacin and neomycin) in bovine milk and bovine, swine and poultry muscle. For sample preparation, an extraction method was developed using trichloroacetic acid and clean up with low temperature precipitation and C18 bulk. Liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) was used to carry out quantitative analysis and liquid chromatography-quadrupole-time of flight-mass spectrometry (LC-QTOF-MS) was used to screening purposes. Both methods were validated according to the European Union Commission Directive 2002/657/EC. Good performance characteristics were obtained for recovery, precision, calibration curve, specificity, decision limits (CCα) and detection capabilities (CCβ) in all matrices evaluated. The detection limit (LOD) and quantification limit (LOQ) were ranging from 5 to 100ngg(-1) and 12.5 to 250ngg(-1), respectively. Good linearity (r)-above 0.99-was achieved in concentrations ranging from 0.0 to 2.0×MRL. Recoveries ranged from 36.8% to 98.0% and the coefficient of variation from 0.9 to 20.2%, noting that all curves have been made into their own matrices in order to minimize the matrix effects. The CCβ values obtained in qualitative method were between 25 and 250ngg(-1). The proposed method showed to be simple, easy, and adequate for high-throughput analysis of a large number of samples per day at low cost.

Simultaneous determination of ten aminoglycoside antibiotics in aquatic feeds by high‐performance liquid chromatography quadrupole‐orbitrap mass spectrometry with pass‐through cleanup

“…To avoid the complicated procedures, mass spectrometry (MS) is an alternative for AGs analysis. Liquid chromatography‐MS (LC‐MS) and liquid chromatography tandem MS (LC‐MS/MS) are widely used methods for single or multi‐AGs residues detection with high selectivity and sensitivity . Recently, high‐resolution MS (HRMS) is another promising approach for multiresidues detection, which is becoming popular due to its superior selectivity in complex sample matrix .…”

“…Liquid chromatography-MS (LC-MS) and liquid chromatography tandemMS(LC-MS/MS)arewidelyusedmethodsforsingleor multi-AGsresiduesdetectionwithhighselectivityandsensitivity. [12][13][14] Recently, high-resolution MS (HRMS) is another promising approach for multiresidues detection, which is becoming popular due to its superior selectivity in complex sample matrix. 15,16 HPLC quadrupole-orbitrap MS (HPLC-Q/Orbitrap MS) is a high-resolution mass spectrometer containingorbitrapmassanalyzer.Thisinstrumentperformsbetter sensitivity and specificity as its high-accurate mass measurement in qualitative and quantitative analysis.…”

Anadolu Manda Sütlerinde Kanamisin Kalıntısının LC-MS/MS İle Belirlenmesi

“…Several detection methods including immunoassays, capillary electrophoresis, high-performance liquid chromatography, gas chromatography, and liquid chromatography-tandem mass spectrometry (LC-MS/MS) were developed for aminoglycoside residue analyses with different sensitivities. However, LC-MS/MS is accepted as the most reliable confirmatory method based on its high sensitivity and accuracy [11,12] .…”

Simultaneous determination of aminoglycoside antibiotics in feeds using high performance liquid chromatography with evaporative light scattering detection

“…Liquid chromatography-mass spectrometry (LC-MS) and liquid chromatography tandem mass spectrometry (LC-MS/MS) analysis appear to be widespread methods for drugs in complex matrices owing to their high sensitivity and selectivity. [16][17][18][19][20][21] However, the determination of AGs in feed using LC-MS and LC-MS/MS has rarely been reported. Furthermore, an evaporative light scattering detector (ELSD) is a sensitive and universal detector used in conjunction with HPLC and is commonly used for the analysis of compounds such as sugars, lipids and novel antibiotics (no UV absorbance) that cannot be detected by a UV detector.…”