Rapid Detection of Per- and Polyfluoroalkyl Compounds in Cosmetics Using Gas Chromatography-Quadrupole/Time of Flight Mass Spectrometry

Abstract

Per- and polyfluoroalkyl substances (PFASs) are a collective term for various artificial fluorinated organic compounds. PFASs not only have hydrophilic functional groups and hydrophobic alkyl side chains, but also have fire resistance, high stability and durability, making them widely used in various industries. PFASs have the characteristics of high toxicity, persistence, bioaccumulation, and long-distance migration of persistent organic pollutants. Different types of PFASs have different harmful effects on biological organisms, and health risks are mostly concentrated in the liver, immune system, and reproductive system. At present, there are many detection methods reported for PFASs in the food and environmental fields, while few methods have been applied for the detection of PFASs in cosmetics. In this work, a method for rapid detection of PFASs in cosmetics was developed by QuEChERS (quick, easy, cheap, effective, rugged, and safe) pretreatment coupled with gas chromatography-quadrupole/time of flight mass spectrometry (GC-Q-TOF MS). Firstly, the extraction solvents, extraction methods, and purification agents were compared, the dosage of purification agents was optimized, and the matrix effect was examined. Eight kinds of volatile PFASs, including two perfluorooctanoic acid esters, four fluoro modified polyacrylates, and two fluoro modified siloxanes in the samples were extracted with 10 mL ethyl acetate, dehydrated by 1 g anhydrous sodium sulfate, and purified by 100 mg graphitized carbon black (GCB) and 50 mg silica gel powder (Si). Target compounds were separated by DB-5MS capillary column (30 m×0.25 mm×0.25 μm), and the mass spectrum was acquired under full scan mode of EI ion source with using external standard method for quantification. The result showed that the work curves of the 8 compounds have good linear relationship, and the correlation coefficient (R2) is greater than 0.997 6 in the range of 5.0-1 000 μg/L. The limits of detection are 20.0 and 200.0 μg/kg, and the limits of quantification are 50.0 and 500.0 μg/kg. The average recoveries at three levels range from 81.4% to 112%, and the relative standard deviations are 1.09%-7.63% (n=6). In total, 105 cosmetic samples purchased from Guangzhou supermarkets and online e-commerce were tested using this method, 8:2FTMAc in 2 samples are detected with 668, 1 004 μg/kg, respectively, indicating that cosmetic samples pose a risk of PFASs contamination, should be taken seriously by regulatory authorities and consumers. This method is high efficiency, sensitive and accuracy, which can provide important basis for the rapid detection and quality control of PFASs compounds in cosmetics.

Keywords

• gas chromatography-quadrupole/time of flight mass spectrometry (gc-q-tof ms)
• rapid detection
• cosmetics
• per- and polyfluoroalkyl compounds (pfass)