Merck
  • Início
  • Resultados da busca
  • Multiresidue method for the determination of pharmacologically active substances in egg and honey using a continuous solid-phase extraction system and gas chromatography-mass spectrometry.

Multiresidue method for the determination of pharmacologically active substances in egg and honey using a continuous solid-phase extraction system and gas chromatography-mass spectrometry.

Food chemistry (2015-02-24)
Abdelmonaim Azzouz, Evaristo Ballesteros
RESUMO

A sensitive, selective, efficient gas chromatography-mass spectrometry method for the simultaneous determination of 22 pharmacologically active substances (antibacterials, nonsteroidal antiinflammatories, antiseptics, antiepileptics, lipid regulators, β-blockers and hormones) in eggs and honey was developed. The sample pretreatment includes precipitation of proteins and lipids with acetonitrile:water (3:2, v/v), centrifugation and continuous solid-phase extraction for cleanup and preconcentration. The proposed method was validated with quite good analytical results including limits of detection of 0.4-3.3 ng/kg for 2g of sample and good linearity (r(2)>0.995) throughout the studied concentration ranges. The recoveries of analytes from real honey and egg samples spiked at concentrations of 15-2,000 ng/kg fell in the range 87-102%, with relative standard deviations from 2.6% to 7.0%. The method was successfully used to determine the target compounds in various types of eggs (hen, quail and duck) and honey samples (flower, forest, acacia, sunflower, clover and pine tree). Two samples of hen eggs bought at supermarkets and one of quail eggs were found to contain florfenicol, pyrimethamine, estrone and 17β-estradiol at levels from 0.095 to 2.7 μg/kg.

MATERIAIS
Número do produto
Marca
Descrição do produto

Sigma-Aldrich
Acetone, ≥99%, meets FCC analytical specifications
Sigma-Aldrich
Acetone, natural, ≥97%
Sigma-Aldrich
Isopropyl alcohol, ≥99.7%, FCC, FG
Supelco
Dehydrated Alcohol, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Ibuprofen, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Hexamethyldisiloxane, viscosity 0.65 cSt (25 °C)
Sigma-Aldrich
Acetone, suitable for HPLC, ≥99.9%
Sigma-Aldrich
Poly(dimethylsiloxane), viscosity 1.0 cSt (25 °C)
Sigma-Aldrich
Methanol, anhydrous, 99.8%
Sigma-Aldrich
Chlorotrimethylsilane, purified by redistillation, ≥99%
Sigma-Aldrich
Acetonitrile solution, contains 0.1 % (v/v) trifluoroacetic acid, suitable for HPLC
Sigma-Aldrich
Acetone, ≥99.5%, ACS reagent
Supelco
Ethanol solution, certified reference material, 2000 μg/mL in methanol
Sigma-Aldrich
Chlorotrimethylsilane, puriss., ≥99.0% (GC)
Sigma-Aldrich
Chlorotrimethylsilane, ≥98.0% (GC)
Supelco
Methanol, analytical standard
Sigma-Aldrich
Chlorotrimethylsilane, produced by Wacker Chemie AG, Burghausen, Germany, ≥99.0% (GC)
Supelco
Acetone, analytical standard
Sigma-Aldrich
Acetone, purum, ≥99.0% (GC)
Supelco
N,O-Bis(trimethylsilyl)trifluoroacetamide with trimethylchlorosilane, for GC derivatization, LiChropur, contains 10% TMCS, 98% (excluding TMCS)
Supelco
Estrone, VETRANAL®, analytical standard
Supelco
N,O-Bis(trimethylsilyl)trifluoroacetamide with trimethylchlorosilane, for GC derivatization, LiChropur, contains 1% TMCS, 99% (excluding TMCS)
Sigma-Aldrich
Estrone, ≥99%
Sigma-Aldrich
Ibuprofen, meets USP testing specifications
Sigma-Aldrich
Ibuprofen, ≥98% (GC)
Sigma-Aldrich
Phenylbutazone
Sigma-Aldrich
Thiamphenicol
Sigma-Aldrich
Mefenamic acid
Sigma-Aldrich
Acetylsalicylic acid, analytical standard
Sigma-Aldrich
Acetylsalicylic acid, ≥99.0%