Dissertação
Desenvolvimento de método para determinação de resíduos de antiparasitários em leite bovino empregando LLE-LTP E LC-MS/MS
Autor
Ribeiro, Lucila Cendon
Institución
Resumen
Milk is one of the most consumed fresh food, considered a nutritionally
complete product. Veterinary drugs are used in order to increase productivity.
However, improper use of these products may result in the presence of
residues in milk. This study aims to develop a method for determination of
antiparasitic residues in bovine milk using fast liquid-liquid low temperature
partitioning (LLE-LTP) method and liquid chromatographic coupled to tandem
mass spectrometry (LC-MS/MS). Different classes were studied for
antiparasitic, such as macrocyclic lactones, pyrethroids, benzimidazoles,
organophosphates, carbamates, among others. The spikes were held
comprising the Maximum Residue Limits (MRLs) of each compound at levels 1-
200 ug L-1. For validation step was adopted the following parameters:
selectivity, linear range, matrix effect, limits of detection (LOD) and quantitation
(LOQ), decision limit (CCα) and detection capability (CCβ), precision, accuracy.
The method was considered valid to 55 antiparasitic and presented LOD from
0.03 to 6.0 μg L-1 and LOQ from 1 to 20 ug L-1. Recoveries were between 70
and 120% with RSD ≤ 20%, that were considered acceptable. The proposed
method was applied to 15 real samples where all samples presented residues
of at least one antiparasitic. Of these, two samples contained cyhalothrin and
nicarbazin residues above the MRL. However, the method was efficient in
determining antiparasitic residues in bovine milk using LLE-LTP and LCMS/
MS, showing good sensitivity and selectivity.