Microwave-assisted extraction and mild saponification for determination of organochlorine pesticides in oyster samples.
A sample-preparation procedure (extraction and saponification) using microwave energy is proposed for determination of organochlorine pesticides in oyster samples. A Plackett-Burman factorial design has been used to optimize the microwave-assisted extraction and mild saponification on a freeze dried sample spiked with a mixture of aldrin, endrin, dieldrin, heptachlor, heptachorepoxide, isodrin, transnonachlor, p, p'-DDE, and p, p'-DDD. Six variables: solvent volume, extraction time, extraction temperature, amount of acetone (%) in the extractant solvent, amount of sample, and volume of NaOH solution were considered in the optimization process. The results show that the amount of sample is statistically significant for dieldrin, aldrin, p, p'-DDE, heptachlor, and transnonachlor and solvent volume for dieldrin, aldrin, and p, p'-DDE. The volume of NaOH solution is statistically significant for aldrin and p, p'-DDE only. Extraction temperature and extraction time seem to be the main factors determining the efficiency of extraction process for isodrin and p, p'-DDE, respectively. The optimized procedure was compared with conventional Soxhlet extraction.
Carro
N
N
Centro de Control de Calidad del Medio Marino. Peirao de Vilaxoán s/n. 36611, Vilagarcía de Arousa, Pontevedra, Spain. ncarro@cccmm.cesga.es
García
I
I
Ignacio
M-C
MC
Llompart
M
M
Yebra
M-C
MC
Mouteira
A
A
D000818:Animals; D002623:Chemistry Techniques, Analytical / Q000379:methods; D006843:Hydrocarbons, Chlorinated; D007306:Insecticides / Q000032:analysis*; D008872:Microwaves; D010125:Ostreidae / Q000737:chemistry*; D013030:Spain
D006843:Hydrocarbons, Chlorinated; D007306:Insecticides