The Study On Detection Technology Of Industrial Perfluorochemicals

Ojective:Perfluorinated compound is a synthetic surfactant, has a unique hydrophobic nature, so these substances have been widely used. They were widely detected in the world, including food samples, environmental samples, biological samples. Existing studies have shown that the toxicity of such substances can not be ignored, for example perfluorooctane sulfonate (perfluorooetaneulfonate, PFOS) has been listed as one of persistent organic pollutants list. For the EU to add these substances prohibited in industrial orders, the establishment of method for the detection of perfluorinated compounds in industrial products is imperative.Method:In this paper, using HPLC-MS/MS combined with the corresponding pre-treatment approaches, methods were established in seven types of industrial products (cosmetics, cleaning agents, fire extinguishing agent, wax, ink. paints, lubricants) for trace analysis of PFCs.1 Seven types of industrial products divided into three categories according to their lipid content, different extraction methods were established:cosmetics, detergents, fire extinguishing agent samples were extracted with methanol by ultrasonic extraction, wax, ink, paint samples were extracted with aqueous solution of tetrahydrofuran by ultrasonic extraction; lubricant samples were extracted by rapid solvent extraction.2 Firstly Oasis WAX cartridges were used for sample clean up:The Oasis WAX cartridges were conditioned by 3mL 0.1% NH4OH in methanol and 3 mL of water.Diluted extracts were transferred onto the WAX SPE cartridges. The cartridges were then washed with 5mL of 25mM acetate buffer at pH4 and 5 mL of methanol. the target analytes were eluted by 3 mL 0.1% NH4OH in methanol.Then clean-up was finished by ENVI-carb cartridges which were conditioned by 3 mL of methanol.The eluates of WAX cartridges passed through the ENVI-carb cartridges.PFCs were eluted with 5mL of 0.1% NH4OH in methanol. Finally, the extracts were anlysized by LC-MS/MS. 3 From linear range, detection limit, recovery, precision in quality control.4 Adopting optimized sample pretreatment methods and instruments conditions on the samples detection.Results:1 In this study, the rate of the extraction method was more than 90%.2 The recoveries of The purification methods were above 95%.3 This method in 10 ng/kg～1000ng/kg within five different concentration level preparation of the blank sample.the experimental determination. Experimental results showed that the concentration and response value good linear relationship. Correlation coefficient (r) are larger than 0.990, response factor relative standard deviation (RSD) 8% to 26%.The detection limit of this method is 5 ng/kg-30ng/kg; limit of quantification was 10ng/kg-50ng/kg; when added levels were 0.005 mg/kg,0.010 mg/kg,0.050 mg/kg, the recoveries of the ten perfluorinated compounds were 70.0%～108.2% and relative standard deviation was 1.8% to 16.6%. The results show that the established method is rapid, high sensitivity and specificity.4 Using liquid chromatography tandem mass spectrometry,70 samples were the detection of perfluorinated compounds, of which 9 samples are detected, and some samples of PFCs exceeding the EU specifications.Conclusion:Thus, in the industrial manufacturing process of our country there are still prohibited use of perfluorinated compounds in the phenomenon. Therefore, the study of industrial goods exports to China is important.