Determination of sulfonamides by packed column supercritical fluid chromatography with atmospheric pressure chemical ionisation mass spectrometric detection

Abstract

Sulfonamide antibiotics are widely used to prevent bacterial infections in livestock, and residues are commonly found in milk and meat. Packed column supercritical fluid chromatography (pSFC) with detection using ultra violet (UV) and atmospheric pressure chemical ionisation (APCI) mass spectrometry (MS) provides a versatile method for the detection and quantification of six major sulfonamides. The APCI mass spectra for all the sulfonamides consisted of protonated molecules at low cone voltages. Increasing the cone voltage led to informative fragmentation patterns, which provided structural information for identification purposes. The pSFC-APCI-MS technique was shown to be linear (r2 > or = 0.999) over the concentration range 0.1-50 micrograms ml-1 using total ion current. The precision and the accuracy of the system and validation of sample preparation are acceptable, with RSD < 2% and relative error 8%. Selected ion monitoring gave detection limits as follows: sulfadiazine 41, sulfamethoxazole 45, sulfamerazine 47, sulfamethizole 59, sulfamethazine 181 and sulfadimethoxine 96 micrograms l-1, which are lower than the amounts permitted in milk products. The APCI pSFC-MS system was shown to have a high degree of reproducibility. The technique was then applied to determine the above sulfonamides in milk. The results obtained show that there are no matrix effects from the milk and that the detection limits remained as stated for the standard solutions.

Hollow fiber supported ionic liquid membrane microextraction for determination of sulfonamides in environmental water samples by high-performance liquid chromatography

“…Sulfonamides (SAs) belong to an important group of bacteriostatic agents used to prevent infections, treat diseases and to promote growth [1]. Due to their wide-ranging activity and low cost, SAs have been widely used in human and veterinary medicine.…”

Otimização e validação de método multirresíduo para determinação de sulfonamidas em camarão cultivado por cromatografia líquida de alta eficiência com detecção por UV

“…Diversos estudos têm reportado os possíveis efeitos carcinogênicos das sulfonamidases; uma pesquisa demonstrou a presença de tumores em roedores ocasionados pelo uso da sulfametazina. [10][11][12][13][14][15] Devido às exigências dos mercados consumidores quanto à segurança alimentar, programas e normas baseados em legislações cada vez mais exigentes vêm sendo criados para fiscalizar os níveis dessas substâncias danosas à saúde humana, estabelecendo-se para as diversas matrizes de origem animal, limites máximos de resíduos (LMR) permitidos. 16,17 No Brasil, o limite máximo de resíduo estabelecido para sulfonamidas em músculo de camarão é 100 µg kg -1 , o mesmo adotado pela Comunidade Europeia.…”

A toxic reagent-free method for normal-phase matrix solid-phase dispersion extraction and reversed-phase liquid chromatographic determination of aldrin, dieldrin, and DDTs in animal fats

“…Their disposal is costly and must be performed with ecological responsibility. Because discharging organic solvent waste is a serious problem, analytical methods should avoid their use [3,4,5].…”