Innovative mixture of salts in the quick, easy, cheap, effective, rugged, and safe method for the extraction of residual macrolides in milk followed by analysis with liquid chromatography and tandem mass spectrometry.

A simple extraction technique has been developed for seven macrolide antibiotics in milk. The procedure involves a modified quick, easy, cheap, effective, rugged, and safe method based on acetonitrile extraction, followed by the addition of a mixture of salts (sodium sulfate, sodium chloride, and potassium carbonate) not yet reported in literature. The method was validated for tylosin and was selective, free of matrix effect, and linear in the range of 0.78-18.75 ng/mL in the final extract, corresponding to 0.125-3 times the maximum residue limit. The limit of detection, limit of quantification, decision limit, and detection capability were, respectively, 0.84, 2.79, 58.4, and 71.7 μg/kg. The overall average recovery at 25, 50, and 75 μg/kg ranged from 89-97%. Repeatability and intermediate precision expressed by relative standard deviations were below 10.5 and 12%, respectively. The extension of the validation for spiramycin, throleandomycin, oleandomycin, roxithromycin, erythromycin, and clarithromycin is under consideration since the procedure proved to be able to efficiently extract all studied macrolides, with recoveries from 74-104% at 50 μg/kg for tylosin, erythromycin, spiramycin, and oleandomycin and 20 μg/kg for throleandomycin, roxithromycin, and clarithromycin.

[1]  I. Galvidis,et al.  Simultaneous separate and group determination of tylosin and tilmicosin in foodstuffs using single antibody-based immunoassay , 2012 .

[2]  P. Delahaut,et al.  Identification and quantification of five macrolide antibiotics in several tissues, eggs and milk by liquid chromatography-electrospray tandem mass spectrometry. , 2001, Journal of chromatography. B, Biomedical sciences and applications.

[3]  D. Hwang,et al.  Multiclass analysis of 23 veterinary drugs in milk by ultraperformance liquid chromatography-electrospray tandem mass spectrometry. , 2012, Journal of chromatography. B, Analytical technologies in the biomedical and life sciences.

[4]  C. Juan,et al.  Determination of macrolide and lincosamide antibiotics by pressurised liquid extraction and liquid chromatography-tandem mass spectrometry in meat and milk. , 2010 .

[5]  F. Ramos,et al.  Development and validation of a multi-residue and multiclass ultra-high-pressure liquid chromatography-tandem mass spectrometry screening of antibiotics in milk , 2013 .

[6]  L. Stolker,et al.  Selectivity in the sample preparation for the analysis of drug residues in products of animal origin using LC-MS , 2013 .

[7]  Steven J Lehotay,et al.  Fast and easy multiresidue method employing acetonitrile extraction/partitioning and "dispersive solid-phase extraction" for the determination of pesticide residues in produce. , 2003, Journal of AOAC International.

[8]  E. J. Threlfall,et al.  Macrolides and lincosamides in cattle and pigs: use and development of antimicrobial resistance. , 2014, Veterinary journal.

[9]  W. Andersen,et al.  Multi-class, multi-residue liquid chromatography/tandem mass spectrometry screening and confirmation methods for drug residues in milk. , 2008, Rapid communications in mass spectrometry : RCM.

[10]  P. Gowik,et al.  Multi-method for the determination of antibiotics of different substance groups in milk and validation in accordance with Commission Decision 2002/657/EC. , 2009, Journal of chromatography. A.

[11]  高野 伊知郎,et al.  LC-MS/MSによる畜産食品中抗生物質のスクリーニング試験法 , 2012 .

[12]  A. G. Frenich,et al.  Multi-residue determination of veterinary drugs in milk by ultra-high-pressure liquid chromatography-tandem mass spectrometry. , 2008, Journal of chromatography. A.

[13]  E. Roets,et al.  Study of the stability of erythromycin in neutral and alkaline solutions by liquid chromatography on poly(styrene-divinylbenzene) , 1995 .

[14]  A. A. Abd El-Aty,et al.  Single-step multiresidue determination of ten multiclass veterinary drugs in pork, milk, and eggs using liquid chromatography with tandem mass spectrometry. , 2015, Journal of separation science.

[15]  Jay P. Graham,et al.  Industrial food animal production, antimicrobial resistance, and human health. , 2008, Annual review of public health.

[16]  A. Laganà,et al.  A simple and rapid confirmatory assay for analyzing antibiotic residues of the macrolide class and lincomycin in bovine milk and yoghurt: hot water extraction followed by liquid chromatography/tandem mass spectrometry. , 2007, Rapid communications in mass spectrometry : RCM.