[Analysis of organochlorine pesticides in buckwheat using pressurized liquid extraction and gas chromatography].
Seven organochlorine pesticides (OCPs) in buckwheat were extracted by a homemade 24 cells auto-pressurized liquid extraction instrument (APLE) and then analyzed by gas chromatography with electronic capture detection. The optimal extraction condition was found to be 100 degrees C and 10 MPa for 5 min with acetone/n-hexane (1:1, v/v) as the extraction solvent. The extraction was performed twice for each sample to obtain complete extraction. The buckwheat was mixed with florisil and active carbon before filling into extraction cells. Concentrated sulfuric acid was used in clean up step of the extractant. The standard mixture of OCPs including alpha-benzene hexachloride (BHC), gamma-BHC, delta-BHC, p, p'-dichloro-diphenyl-dichloroethylene (p,p'-DDE), p,p'-dichloro-diphenyl-dichloroethane (p, p'-DDD), o, p-dichloro-diphenyl trichloro-ethane (o,p-DDT), p,p'-DDT was used for the identification and quantification in gas chromatographic analysis. The absolute recoveries of the 7 organochlorine pesticides were between 68%-126% with the relative standard deviations lower 14.7%. The detection limits were between 0.051 - 0.18 ng/g. The relative recoveries were as high as 116%-148% compared with Soxhlet extraction. It shows that the recoveries of APLE are much better than Soxhlet extraction, and the time of extraction for APLE is only about 15 min which is much less than conventional extraction methods.
Lian
Mei
M
Dalian Institute of Chemical Physics, the Chinese Academy of Sciences, Dalian 116023, China.
Xu
Feng
F
Guan
Wenna
W
Xu
Yuan
Y
Guan
Yafeng
Y
D002849:Chromatography, Gas; D019612:Fagopyrum / Q000737:chemistry*; D005504:Food Analysis / Q000295:instrumentation / Q000379:methods*; D006843:Hydrocarbons, Chlorinated / Q000032:analysis* / Q000302:isolation & purification*; D057230:Limit of Detection; D016014:Linear Models; D010573:Pesticide Residues / Q000032:analysis* / Q000302:isolation & purification*; D011312:Pressure; D015203:Reproducibility of Results
D006843:Hydrocarbons, Chlorinated; D010573:Pesticide Residues