Determination of anxiolytic veterinary drugs from biological fertilizer blood meal using liquid chromatography high‐resolution mass spectrometry

Abstract

A liquid environment-friendly agricultural material originating from animal blood, blood meal, was employed to detect anxiolytic veterinary drugs using a combination of liquid-liquid extraction (LLE) and positive electrospray ionization Orbitrap mass spectrometry. Every positive ion of the analytes was consistent with [M+H](+) , and the accurate mass analysis and mass spectral filtration with a 2-ppm mass tolerance window were applied to identify and quantitate the analytes and metabolites. The developed LLE method was validated with the lowest calibrated level, linearity (r(2) ), recovery, repeatability and the within-laboratory reproducibility, which were in the ranges of 0.3-1 µg/L, 0.9963-0.9995, 48.3-117.5%, 1.1-12.6% and 2.3-15.7%, respectively. The LLE method was compared with a solid-phase extraction (SPE) method; however, its recoveries were <70% for most of the analytes despite good repeatability of 1.2-7.4%. The analytes and the ascertained acepromazine, azaperone and xylazine metabolites were monitored in four actual liquid blood meal samples, and none of the targeted compounds were observed.

Development of a method for the determination of sedatives in bovine and porcine urine and kidneys by liquid chromatography–tandem mass spectrometry

“…After optimisation of the analytes and selection of appropriate characteristic ions, we optimised the chromatographic conditions. Chromatographic separation for these substances is usually performed using C 18 - or octylsilane (C 8 )-filled columns of different lengths ( 1 , 3 , 4 , 8 , 25 ).…”

“…The fast, cheap and simple character of the QuEChERS technique and its good reproducibility recommended this method for the analysis of these compounds. The most commonly used reagents to extract the tested sedatives are acetonitrile, ethyl acetate, trifluoroacetic acid and methanol ( 1 , 4 , 8 , 28 , 29 , 36 , 40 ). Acetonitrile and ethyl acetate gave the best recoveries; therefore, these two solvents were considered during the development of the method.…”

“…The most commonly used extraction methods for this group of compounds are liquid–liquid extraction (LLE), solid-phase extraction (SPE), and QuEChERS (quick, easy, cheap, effective, rugged, and safe). Liquid–liquid extraction is extraction with acetonitrile, methanol, trifluoroacetic acid and ethyl acetate; additionally, ammonia, ammonium formate or acetic acid may be used ( 1 , 4 , 8 , 28 , 29 , 36 , 40 ). A modification of LLE extraction is QuEChERS, in which the sample is additionally purified using octadecylsilane (C 18 ) and primary and secondary amine (PSA) sorbents ( 38 , 41 ).…”

“…A more conservative approach granting better purification of the extract but requiring longer sample preparation time is the SPE technique. In this technique, the most commonly used columns are those containing silica, C 18 , and the polymeric reversed-phase sorbent ( 1 , 4 , 22 , 35 , 38 ). The difficulty of determining these substances in kidney tissue prompted some authors to test the possibility of combining the LLE technique with SPE for better purification of the extracts ( 1 , 38 ).…”

“…Mass spectrometry's specificity made it possible to confirm or possibly exclude the tested substance. This technique accelerated the development of analytical methods and the determination of residues of these substances in biological material (1,4,7,20,23,25,35,36,38,39). Better possibilities for the determination of these substances resulted in the simplification of sample preparation.…”