Microwave-assisted extraction and mild saponification for determination of organochlorine pesticides in oyster samples

被引:24
作者
Carro, N
García, I
Ignacio, MC
Llompart, M
Yebra, MC
Mouteira, A
机构
[1] Ctr Control Calidad Medio Marino, Vilagarcia De Arousa 36611, Pontevedra, Spain
[2] Fac Quim, Dept Quim Analit Nutr & Bromatol, Santiago De Compostela 15706, Spain
关键词
microwave-assisted extraction (MAE); microwave-assisted mild saponification (MAMS); organochlorine pesticides; oyster sample; gas chromatography-mass spectrometry;
D O I
10.1007/s00216-002-1437-1
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
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.
引用
收藏
页码:547 / 553
页数:7
相关论文
共 24 条
[1]   SUPERCRITICAL-FLUID EXTRACTION OF ANALYTES FROM ENVIRONMENTAL-SAMPLES - A REVIEW [J].
BARNABAS, IJ ;
DEAN, JR ;
OWEN, SP .
ANALYST, 1994, 119 (11) :2381-2394
[2]   OPTIMIZATION OF SOLID-PHASE MICROEXTRACTION CONDITIONS FOR DETERMINATION OF PHENOLS [J].
BUCHHOLZ, KD ;
PAWLISZYN, J .
ANALYTICAL CHEMISTRY, 1994, 66 (01) :160-167
[3]  
Carro N, 1999, J MICROCOLUMN SEP, V11, P544, DOI 10.1002/(SICI)1520-667X(1999)11:7<544::AID-MCS7>3.0.CO
[4]  
2-3
[5]   AEROMONAS-HYDROPHILA INFECTIONS OF SKIN AND SOFT-TISSUE - REPORT OF 11 CASES AND REVIEW [J].
GOLD, WL ;
SALIT, IE .
CLINICAL INFECTIOUS DISEASES, 1993, 16 (01) :69-74
[6]  
GONZALEZQUIJANO A, 1996, PESCA ALIMENTACION, V27, P212
[7]   EXTRACTION OF ORGANIC POLLUTANTS FROM ENVIRONMENTAL SOLIDS WITH SUBCRITICAL AND SUPERCRITICAL WATER [J].
HAWTHORNE, SB ;
YANG, Y ;
MILLER, DJ .
ANALYTICAL CHEMISTRY, 1994, 66 (18) :2912-2920
[8]   Comparison of ASE and SFE with Soxhlet, sonication, and methanolic saponification extractions for the determination of organic micropollutants in marine particulate matter [J].
Heemken, OP ;
Theobald, N ;
Wenclawiak, BW .
ANALYTICAL CHEMISTRY, 1997, 69 (11) :2171-2180
[9]  
Jocelyn Pare J. R., 1995, Microwave-Assisted Extraction from Materials Containing Organic Matter, Patent No. 5458897
[10]  
Kingston H.M., 1998, INTRO MICROWAVE SAMP