A novel microwave-assisted and temperature-controlled headspace solid-phase microextraction ( MATC-HS-SPME ) couple to gas chromatography-negative ion chemical ionization mass spectrometry ( GC-MS-NCI ) method was developed for the determination of six pyrethroids, including fenpropathrin, ?-cyhalothrin, cypermethrin, flucythrinate, fenvareate and deltamethrin, in aqueous samples. The method is based on the heating of aqueous sample with microwave radiation to the elevated temperature to evaporate analysts to the headspace where the temperature is controlled by a cooling circulate system. The purpose of this work was to develop a rapid, simple, efficient, economical and environmental friendly method for the simultaneous extraction of 6 synthetic pyrethroids in water samples. Factors which might affect extraction efficiency, such as microwave power, type of SPME fiber, extraction time, headspace temperature, sample agitation rate, salt concentration, and pH of the sample were investigated. Under the optimum condition (microwave power at 250 watts, headspace temperature at 15oC, extraction time for 30 min, agitation at high level, sodium concentration of 0.5 M, and pH 4), good linearity was obtained in a range of 0.100 � 10 ng/ml for the six analytes with correlation coefficient ?2> 0.994. The method detection limits were between 2.1 � 6.0 pg/ml. The developed technique was applied to the real samples with satisfied extraction efficiency, precision and accuracy.

Microwave-assisted and temperature-controlled headspace solid-phase microextraction coupled with gas chromatography-negative ion chemical ionization mass spectrometry for the determination of pyrethroids in aqueous samples

244th National Meeting (2012)

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