Temperature-controlled headspace solid phase microextraction combined with gas chromatography-mass spectrometry for determination of phthalate in aqueous samples

• Main Authors: Yu-Chieh Wang, 王毓傑
• Other Authors: Youn-Yuen Shu
• Format: Others
• Language: zh-TW
• Published: 2013
• Online Access: http://ndltd.ncl.edu.tw/handle/54776491777803161588

碩士 === 國立高雄師範大學 === 化學系 === 101 === We developed a new method which involves temperature-controlled headspace solid phase microextraction combined with gas chromatography-mass spectrometry(GC-MS). This method is used to determine six common phthalate in aqueous samples. In this study involving temperature-controlled headspace solid phase microextraction, Purge-Assisted and Temperature Controlled Headspace Solid-Phase Microextraction (PATC-HS-SPME) and Microwave-Assisted and Temperature Controlled Headspace Solid-Phase Microextraction (MATC-HS-SPME) are used as preconcentration. GC-MS is used for quantitative and qualitative. For PATC-HS-SPME, a 2 cm fiber is used which is coated with DVB/CAR/PDMS. We extracted an aqueous solution with 3 g salt at pH 4, stirring at a speed of 500 rpm, with extraction temperature of 180 ℃, cooling temperature to 20 ℃, extraction position 1 cm and the nitrogen flow rate of 50 mL/min for 1 hour. The resulting detection limit is ranged from 0.04 to 0.18 ng / mL, the correlation coefficient ranged from 0.9922 to 0.9954 and the relative standard deviations ranged from 1.4% to 22.4%. For MATC-HS-SPME, a 2 cm fiber is used which is coated with DVB/CAR/PDMS. We extracted an aqueous solution with 3 g salt at pH 4 in stirring speed 800 rpm, microwave power 250W,cooling temperature to 20 ℃ for 1 hour. The resulting detection limits ranged from 0.03 to 0.13 ng / mL, the correlation coefficient ranged from 0.9916 to 0.9985 and the relative standard deviations ranged from 2.4% to 18.9% We was successfully developed using temperature-controlled headspace solid phase microextraction instead of organic solvents for preconcentration. It is combined with GC-MS resulting high sensitivity and reproducibility. This can be widely used to detect for phthalates in aqueous samples.