Targeted Analysis of Veterinary Drugs in Food Samples by Developing a High-Resolution Tandem Mass Spectral Library

Abstract

Veterinary drug residues present in foods can pose severe health threats to the population. The present study aims to develop a high-resolution mass spectral library of 158 veterinary drugs of 16 different classes for their rapid identification in food samples through liquid chromatography−high-resolution electrospray ionization-tandem mass spectrometry (LC-HR-ESI-MS/MS). Standard drugs were pooled according to their log P values and exact masses before analysis. Spectra were collected at system automated collision energy, i.e., of 25−60 eV and four predetermined collision energies (10, 20, 30, and 40 eV) for each compound using a schedule precursor list of [M + H] + , [M + Na] + , and [M + NH 4 ] + ions. The utility of the developed database was checked by analyzing food samples. A total of 17 veterinary drugs based on the reference standard retention times (RTs), HR-MS spectra, and MS/MS spectra were identified in the analyzed samples. Moreover, five veterinary drugs were selected for quantitative analysis, including doxycycline hyclate, lincomycin, sulfasalazine, moxifloxacin, and diphenoxylate, using liquid chromatography−ion trap mass-spectrometry (LC-IT-MS). Concentrations of the drug were obtained to vary from 0.0805 to 0.9731 mg/kg in food samples and were found to be exceeded in most of the cases as per the maximum residue levels described by Food and Agriculture Organization (FAO)/World Health Organization (WHO). The MS data were submitted to the MetaboLights online database (MTBLS2914). This study will help in the high-throughput screening of multiclass veterinary drugs in foodstuffs.

Fungicide Metabolite MS2 Spectral Libraries for Comprehensive Human Biomonitoring

“…The major advantages of the workflow are (1) it uses the feature abundance in SG normalized mice urine for improved quantification to select suspect metabolite candidates, (2) it combines two complementary chromatographies, and positive and negative ionization modes to cover the polar metabolites in urine produced via phase I and II metabolism (e.g., sulfation, glucuronidation), (3) it can be applied to any chemical and is not limited to the phase I and II metabolites. In addition to traditional spectral libraries constructed using chemical standards, , considerable progress has recently been made in constructing metabolite MS2 libraries of chemicals of concern using human liver S9 incubations for nontargeted screening. , Such approaches are performed on a compound-by-compound basis and include dedicated sample preparation (e.g., extraction and glucuronidase treatment) and yield curated libraries with structure annotation based on MS2 fragmentation patterns. With the same goal to improve nontargeted suspect screening, we pursued the creation of more comprehensive, suspect metabolite MS2 libraries resulting from mammalian whole body metabolism (vs S9 preparations).…”

“…Despite extensive research on fungicides, a number of reported metabolites are not in chemical databases such PubChem (e.g., tebuconazole–COOH (Figure C), tebuconazole glucuronides and sulfates), which impedes their detection in nontargeted data sets. Furthermore, even libraries constructed using chemical standards, as for example veterinary drugs, are not readily available despite linking to public repositories. We have deposited the mice urinary data sets in the MetaboLights repository and made the MS2 spectral libraries available in MoNA .…”

High-capacity boronate affinity-based template-immobilized surface imprinted silica nanoparticles for rapid, selective, and efficient extraction and determination of lincomycin in milk and chicken

“…Thus far, a variety of analytical methods have been used to evaluate Lin in different real samples including GC-MS (Tao et al, 2011), LC-MS (Khadim et al, 2023), LC-MS/MS (Fernandes-Cunha et al, 2015;Maddaleno et al, 2019;Du et al, 2021;Li et al, 2021), and immunoassay (Zhou et al, 2014;Cao et al, 2015). Although these methods have many advantages, especially good sensitivity and accuracy, most of them suffer from several drawbacks, such as costly instruments, complicated sample preparation, long time consumption, and poor storage stability.…”