Development and validation of analytical method for sulfonamide residues in eggs by liquid chromatography Tandem Mass Spectrometry based on the Comission Decision 2002/657/EC

Abstract

A técnica de cromatografia líquida acoplada a um espectrômetro de massas com ionização "electrospray" (LC-ESI-MS/MS) foi usada para a determinação simultânea de resíduos de dez sulfonamidas (SAs: sulfacetamida, sulfatiazol, sulfamerazina, sulfametazina, sulfametoxipiridazina, sulfametazol, sulfacloropiridazina, sulfametoxazol, sulfadimetoxina e sulfaquinoxalina) em ovos. As amostras foram preparadas por precipitação das proteínas com acetonitrila seguida por extração em fase sólida. Após remoção do solvente e reconstituição, os extratos finais foram injetados no LC-ESI-MS/MS no modo positivo para todas as sulfonamidas. O método validado resultou em recuperação entre 87 e 116% com desvios padrão relativo entre 8,5 e 27,2%, CCa entre 101,0 e 122,1 ng g -1 e CCb entre 114,5 e 138,8 ng g -1 . O método analítico, no qual foram utilizadas amostras fortificadas, foi validado baseado na Decisão da Comissão 2002/657/CE.Liquid chromatography-electrospray ionization -tandem mass spectrometry (LC-ESI-MS/MS) was used to simultaneous determination of ten sulfonamide (SAs) residues (sulfacetamide, sulfathiazole, sulfamerazine, sulfamethazine, sulfamethoxypyridazine, sulfamethizole, sulfachloropyridazine, sulfamethoxazole, sulfadimethoxine and sulfaquinoxaline) in eggs. Samples were extracted with acetonitrile and the supernatants were cleaned up by solid phase extraction. After solvent evaporation and reconstitution, aliquots of the final extracts were injected into a LC-ESI-MS/MS in positive mode for all sulfonamides. The validated method resulted in recoveries ranging between 87 and 116% with relative standard deviations between 8.5 and 27.2%, CCa between 101.0 and 122.1 ng g -1 , and CCb between 114.5 and 138.8 ng g -1 . The analytical method, using fortified samples, was validated based on the Commission Decision 2002/657/EC.

Method Development and Validation for Quantification of Sulfamethoxazole in Human plasma by UPLC-MS/MS

“…However a method for determining Sulfamethoxazole and Trimethoprim in rat plasma using Estazolam as Internal standard was proposed in LCMS (Wang et al, 2012). In LCMS, ten sulfonamides in eggs were studied (de la Cruz et al, 2011). Sulfamethoxazole and Trimethoprim were quanti ied by SPE (Solid Phase Extraction) method and compared two methods ef iciency such as LC with UV and MS detection (Bedor et al, 2008).…”

Voltammetric Determination of Sulfonamides with a Modified Glassy Carbon Electrode Using Carboxyl Multiwalled Carbon Nanotubes

“…Currently, various methods, such as liquid chromatography, [6][7][8][9][10][11][12] capillary electrophoresis, [13][14][15][16] gas chromatography (GC), [17][18][19] micellar electrokinetic capillary chromatography, [19][20][21][22] and liquid mass chromatography, 23,24 have been proposed for analyzing SAs residue in food. These techniques have been proved to be suitable and sensitive for SAs detection.…”

Validated HPLC Method to Simultaneously Determine Amprolium Hydrochloride, Sulfaquinoxaline Sodium and Vitamin K3 in A.S.K Powder on ZIC-HILIC Column

“…There are different non-chromatographic and chromatographic methods, particularly RP-HPLC and ion-pair RP-HPLC, which report about the assay of each active ingredient individually or when present in combinations with other ingredients [1][2][3][4][5][6][7][8][9][10][11][12][13][14][15][16][17]. Some of these…”