Method Validation of Phthalates and Polycyclic Aromatic Hydrocarbons in Edible Oil using Isotope Dilution Gas Chromatography-Time of Flight Mass Spectrometry

Title
Method Validation of Phthalates and Polycyclic Aromatic Hydrocarbons in Edible Oil using Isotope Dilution Gas Chromatography-Time of Flight Mass Spectrometry
Authors
박현미이선화정민지오민석박경수
Keywords
Method Validation; Phthalates and Polycyclic Aromatic Hydrocarbons; Oil; Edible oils; GC-TOF MS
Issue Date
2012-08
Publisher
2012APWC
Abstract
A method was developed for the simultaneous determination of four phthalates(Dibutyl phthalate, Benzyl butyl phthalate, Diethylhexyl adipate, Diethylhexyl phthalate) and eight polynuclear aromatic hydrocarbons (PAHs; Benzo[a]anthracene, Chrysene, Benzo[b]fluoranthene, Benzo[k]fluoranthene, Benzo[a]pyrene, Indeno[1,2,3-cd]pyrene, Benzo[g,h,i]perylene, Dibenz[a,h]anthracene) in edible oil. The analytical procedure was based on the liquid-liquid extraction and solid phase extraction for clean up. It was difficult and important to select the solvent because matrix was oil. When compared with various extraction solvent, acetonitrile 15mL was appropriate in liquid-liquid extraction. For removing impurity and lipid, florisil glass cartridge and hexane-dichloromethane (1:1, v/v, 15mL) for elution solvent in solid phase extraction were used. Analytes were determined by gas chromatography with mass spectrometric detection using isotope dilution method for reduce matrix effect. Twelve kinds of deuterated isotope internal standard was used because isotope dilution method was coupled with analytes. In GC/TOFMS; Oven temperature gradient was optimized to effectively separate twelve analytes and twelve internal standard and mass spectrometry condition and base peak ion was optimized to exactly quantify analytes,. Validation study for established method were carried out by evaluate linearity, method limit of detection, method limit of quantification, accuracy and precision. This method could be suitable to quantitate phthalates and PAHs in edible oils simultaneously.
URI
http://pubs.kist.re.kr/handle/201004/43006
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KIST Publication > Conference Paper
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