Determination of Macrocyclic Lactone Drug Residues in Animal Muscle by Liquid Chromatography/Tandem Mass Spectrometry

Abstract

A robust, credible, and practical multiresidue method based on liquid chromatography/tandem/mass spectrometry (LC/MS/MS) was developed for the simultaneous determination of 9 macrocyclic lactone drugs (abamectin B1a, doramectin, erythromycin, ivermectin B1a, josamycin, kitasamycin, roxithromycin, tilmicosin, and tylosin A) in bovine, porcine, chicken, and sheep muscles. The drugs were extracted with acetonitrile, and the extracts were defatted with n-hexane and further cleaned up on a C18 solid-phase extraction cartridge. LC/MS/MS data acquisition was achieved by using the multiple-reaction monitoring (MRM) mode, i.e., 2 transitions, to provide a high degree of sensitivity and repeatability. Matrix-matched standard calibration curves were used to achieve the best accuracy of the method by compensating for the matrix effect. The calibration graphs were linear (r >0.998) from 10 to 1000 ng/mL for erythromycin, josamycin, kitasamycin, roxithromycin, tilmicosin, and tylosin, and from 5 to 250 ng/mL for abamectin, doramectin, and ivermectin. The average recoveries of the 9 drugs were between 64.5 and 105, calculated by using matrix-matched calibration, with relative standard deviation values ranging from 1.6 to 14. The limits of detection were 0.1 g/kg for erythromycin, josamycin, roxithromycin, and tylosin; 0.2 g/kg for tilmicosin and kitasamycin; and 0.5 g/kg for abamectin, doramectin, and ivermectin. For confirmation, the MRM ratios for the 9 drug residues in the samples and the solvent were evaluated and found to be within the ratio criteria set by the guidelines of the European Union.

Simultaneous determination of ten macrolides drugs in feeds by high performance liquid chromatography with evaporation light scattering detection

“…The Oasis HLB cartridge, 23 Bond Elut-C 18 cartridge, 14,24,25 and Oasis MCX cartridge, 26,27 have been reported to cleanup macrolides drugs in extracts of feeds. Thus, three types of cartridges were applied for purifying the extracts of three solvents above, respectively.…”

“…Numerous methods have been developed for the determination of macrolides drugs in animal tissues, urine and feeds by liquid chromatography (LC) with ultraviolet (UV), electrochemical or uorimetric detection, [6][7][8][9][10] and by liquid chromatography-mass spectrometry (LC-MS) or liquid chromatography-tandem mass spectrometry (LC-MS/MS). [11][12][13][14] However, most of macrolides drugs have weak UV absorbance in the low wavelength range as it lacks a suitable chromophore. 15 Therefore, a sensitive and selective UV detection of this group is difficult.…”

Distribuição de resíduos de ivermectina e eprinomectina em diferentes tecidos bovinos e em produtos cárneos enlatados termicamente processados

“…No que se refere a métodos qualitativos ou semi quantitavos, os primeiros anticorpos monoclonais para imunoensaios de avermectinas foram relatados por Schmidt et al (1990). Crooks et al (1998) GRIMALT et al, 2005;HE et al, 2009;HERNANDO et al, 2007;HOU et al, 2006 (KINSELLA et al, 2009;INOUE et al, 2009;WHELAN et al, 2010 (c) Conhecer o nível de correlação entre os resultados de concentração de resíduos no fígado e no músculo (cortes cárneos comerciais);…”