Analytical method for the determination of usually prescribed antibiotics in human nails using UHPLC-MS/MS. Comparison of the efficiency of two extraction techniques

Abstract

Antibiotics are a group of drugs used for the treatment of bacterial diseases. They are used in both human and veterinary medicine and, although they are not permitted, they are sometimes used as growth promoters. The present research compares two extraction techniques: ultrasound-assisted extraction (UAE) and microwave-assisted extraction (MAE) in order to evaluate their efficiency in the determination of 17 usually prescribed antibiotics in human nails. The extraction parameters were optimized using multivariate techniques. Once both techniques were compared, MAE was selected as optimal due to its greater experimental practicability together with the better extraction efficiencies it provides. Target analytes were detected and quantified by ultra-high performance liquid chromatography with tandem mass spectrometry detection (UHPLC-MS/MS). The run time was 20 min. The methodology was then successfully validated, obtaining acceptable analytical parameters according to the guide used. Limits of detection were between 0.3 and 3 ng g−1 and limits of quantification were in the range from 1.0 to 4.0 ng g−1. Recovery percentages ranged from 87.5% to 114.2%, and precision (in terms of standard deviation) was less than 15% in all cases. Finally, the optimized method was applied to nails taken from 10 volunteers and the results revealed the presence of one or more antibiotics in all the samples examined. The most commonly found antibiotic was sulfamethoxazole, followed by danofloxacin and levofloxacin. The results demonstrated, on the one hand, the presence of these compounds in the human body and, on the other hand, the suitability of nails as a non-invasive biomarker of exposure.