Screening of Phthalates Plasticizers in Plastic Toys by Ultra-performance Liquid Chromatography-Hybrid Quadrupole Time-of-flight Mass Spectrometry

KeyWord:phthalates  plasticizers  solid phase extraction  ultra performance liquid chromatography-hybrid quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF MS)  plastic toys  screening

Abstract:

      An analytical method was developed for the rapid screening and quantitative detection of fifteen phthalates(PAEs) plasticizers in plastic toys by ultra performance liquid chromatography-hybrid quadrupole time of flight mass spectrometry(UPLC-Q TOF MS).Plastic toy samples of different matrixes were extracted by a solvent dissolution-ultrasound extraction-precipitation seperation,cleaned up with a graphite carbon solid phase extraction column and concentrated by rotary evaporation and nitrogen blowing,then separated on a C18 column(2.1 mm¡Á50 mm,1.7 ¦Ìm) by gradient elution,and detected in positive electrospray ionization(ESI+) and information dependent acquisition(IDA) MS/MS mode.The qualitative analyses for fifteen PAEs were performed by the synergic combination of the accurate m/z of TOF MS,isotopic distribution,retention time and library search results.The quantitative analyses were performed using the peak area of the extracted m/z of TOF MS.Experimental results demonstrated that a favorable mass accuracy less than 3 ppm was obtained for fifteen PAEs,and good linearities(r2>0.996) were observed in the respective concentration ranges.The limits of detection(LODs) and limits of quantitation(LOQs) were in the ranges of 4.66-11.69 ¦Ìg/kg and 13.04-30.71 ¦Ìg/kg,with intra-day and inter-day(n=7) precision less than 3.8% and 6.7%,respectively.The recoveries at three spiked levels ranged from 80.5% to 108.3%,with relative standard deviations(RSDs,n=6) of 0.4%-12.3%.The present method was practically used to detect butyl benzyl phthalate in a plastic toy.This method was proved to be accurate,efficient and specific,and could be applied for the inspection of commercial plastic toys.