Investigating POPS In Skin Toner By SBSE-GC/MS And SPME-GC/MS

With the improvement of people’s living standard, Cosmetics havegradually become people’s daily necessities. Thus, cosmetics safetyconcerns are getting more and more attention. In this paper, Threemethods for detecting PCBs and PBDEs residue in skin toner sampleswere presented, including pre-treatment procedure and detectiontechnique. The optimized methods were fast, accurate, low pollution,high sensitivity and content with Green Analytical Chemistry’srequirement.First, a method based on ionic liquid-assistant solid phasemicroextraction coupled with gas chromatography-massspectrometry(SPME-GC/TOFMS) had been developed to determineseven polychlorinated biphenyls (PCB-28,52,101,118,138,153,180) inskin toner. Also, the SPME-GC/TOFMS procedure was optimized onsome factors, such as type of fiber, extraction temperature and time,concentration and volume of ionic liquid. Furthermore, the developedmethod was validated by the recovery, coefficient, and reproducibility(relative standard deviation (RSD), n=3). Recoveries for all PCBs were between68.9%and104.7%at spiking levels (200pg/g,5000pg/g,20000pg/g). The developed method was linear at concentrations within100pg/g~40000pg/g, with coefficients of correlation higher than0.999,The LODs were100pg/g~200pg/g. Finally，the method was used to testreal samples with reliable results.Second, a method based on stir bar sorptive extraction coupled withthermal desorption-gas chromatography-mass spectrometry(SBSE-TD-GC/TOFMS) had been developed to determine sevenpolychlorinated biphenyls (PCB-28,52,101,118,138,153,180) in skintoner. Also, the SBSE-TD-GC/TOFMS procedure was optimized onsome factors, such as cold injection temperature, thermodesorption time,extraction time and extraction solvent. Furthermore, the developedmethod was validated by the recovery, coefficient, and reproducibility(relative standard deviation (RSD), n=3). Recoveries for all PCBs werebetween74.1%and106.8%at spiking levels (60pg/g，200pg/g，1000pg/g). The developed method was linear at concentrations within60pg/g~1000pg/g, with coefficients of correlation higher than0.996, TheLODs were5pg/g~60pg/g. Finally，the method was used to test realsamples with reliable results.Third, a method based on ionic liquid-assistant solid phasemicroextraction coupled with gas chromatography-mass spectrometry(SPME-GC-QQQ) had been developed to determine four polybrominated diphenyl ethers (BDE-2,13,28,66) in skin toner. Also, theSPME-GC-QQQ procedure was optimized on some factors, such as typeof fiber, extraction temperature and time, concentration and volume ofionic liquid. Furthermore, the developed method was validated by therecovery, coefficient, and reproducibility (relative standard deviation(RSD), n=3). Recoveries for all PCBs were between81.5%and111.3%at spiking levels (500pg/g,20000pg/g,500000pg/g). The developedmethod was linear at concentrations within200pg/g~500000pg/g, withcoefficients of correlation higher than0.996, The LODs were100pg/g~200pg/g.