Systematical method for polyacrylamide and residual acrylamide detection in cosmetic surgery products and example application.
BACKGROUND
In this paper, the authors presented a case of acrylamide poisoning in a middle-aged woman who had underwent unsuccessful cosmetic surgery six years earlier. The victim was told that the product that had been injected into her face was Restylane®, which mainly contained sodium hyaluronate and was the first and only Food and Drug Administration (FDA)-approved dermal filler for lip enhancement in the USA for more than 20 years. Widespread facial infections occurred several years post-injection; finally, the victim had to undergo removal surgery. Acrylamide poisoning was strongly suspected based on the victim's clinical manifestation. The product that had been injected into the victim's face was probably polyacrylamide hydrogel-based product, which had been prohibited by the State Food and Drug Administration (SFDA) in China in 2006. To confirm this suspicion, a systematical method was established to differentiate varieties of cosmetic surgery products and identify residential acrylamide.


METHODS
The removed objects, original products and a certified reference sample of Restylane® were collected for examination. A direct microscopic examination was applied as a rapid screening method. Fourier transform infrared (FTIR) microspectroscopy analysis was subsequently performed to distinguish the main components from each sample. Automated solid phase extraction, ultra high performance liquid chromatography (SPE UHPLC) analysis was ultimately utilised and optimised to detect the residual acrylamide. Chromatographic separation was achieved on an ACQUITY UHPLC HSS T3 column. The mobile phase consisted of 0.01% aqueous formic acid solution and acetonitrile. The tunable UV (TUV) detection wavelength was at 202nm.


RESULTS
The microscopic examination indicated that different samples had different morphological characteristics, depending on their main components. The FTIR spectrum showed that different polymers could be distinguished according to the CO stretching vibration (1655cm(-1)), NH bending vibration (1540cm(-1)) and CO stretching vibration (1078 and 1045cm(-1)). The UHPLC results demonstrated that the calibration curve was linear in the range of 0.5-20.0μg/mL, with a correlation coefficient of 0.999. The average recoveries of the method were 99-107% with an RSD of 1.6-6.3%. The detection limit was 0.1μg/mL (S/N=3). The analytical time was 6min per sample. Acrylamide was detected in the allegedly Restylane® injection.


CONCLUSIONS
This systematical method provides a rapid, accurate and sensitive determination of polyacrylamide and residual acrylamide. The microscopic and FTIR spectroscopic examinations help to verify the existence of polyacrylamide quickly and easily. The optimised SPE UHPLC-TUV method offers a simpler and more sensitive approach to confirm the amount of acrylamide, comparing to the methods in the literature.
China University of Political Science and Law, Beijing, China. judie0505@gmail.com
Yuanfeng
Y
Wang
Ran
R
Du
Tianshui
T
Yu
Acrylamide; FTIR micro spectroscopy; Polyacrylamide; UHPLC