MSPD procedure for determining buprofezin, tetradifon, vinclozolin, and bifenthrin residues in propolis by gas chromatography-mass spectrometry.
A simple and effective extraction method based on matrix solid-phase dispersion (MSPD) was developed to determine bifenthrin, buprofezin, tetradifon, and vinclozolin in propolis using gas chromatography-mass spectrometry in selected ion monitoring mode (GC-MS, SIM). Different method conditions were evaluated, for example type of solid phase (C(18), alumina, silica, and Florisil), the amount of solid phase and eluent (n-hexane, dichloromethane, dichloromethane-n-hexane (8:2 and 1:1, v/v) and dichloromethane-ethyl acetate (9:1, 8:2 and 7:3, v/v)). The best results were obtained using 0.5 g propolis, 1.0 g silica as dispersant sorbent, 1.0 g Florisil as clean-up sorbent, and dichloromethane-ethyl acetate (9:1, v/v) as eluting solvent. The method was validated by analysis of propolis samples fortified at different concentration levels (0.25 to 1.0 mg kg(-1)). Average recoveries (four replicates) ranged from 67% to 175% with relative standard deviation between 5.6% and 12.1%. Detection and quantification limits ranged from 0.05 to 0.10 mg kg(-1) and 0.15 to 0.25 mg kg(-1) propolis, respectively.
dos Santos
Thaíse Fernanda Santana
TF
Departamento de Química, Universidade Federal de Sergipe, Av. Marechal Rondon s/no, Jardim Rosa Elze, Cep. 49100-000, São Cristóvão, SE, Brazil.
Aquino
Adriano
A
Dórea
Haroldo Silveira
HS
Navickiene
Sandro
S
D002138:Calibration; D008401:Gas Chromatography-Mass Spectrometry; D006843:Hydrocarbons, Chlorinated / Q000032:analysis* / Q000737:chemistry; D015394:Molecular Structure; D010080:Oxazoles / Q000032:analysis* / Q000737:chemistry; D011429:Propolis / Q000032:analysis* / Q000737:chemistry; D011722:Pyrethrins / Q000032:analysis* / Q000737:chemistry; D013829:Thiadiazines / Q000032:analysis* / Q000737:chemistry
D006843:Hydrocarbons, Chlorinated; D010080:Oxazoles; D011722:Pyrethrins; D013829:Thiadiazines; C083997:buprofezin; C099952:bifenthrin; D011429:Propolis; C025643:vinclozolin; C005807:tetradifon