title: Identification and quantification of seven volatile n-nitrosamines in cosmetics using gas chromatography/chemical ionization-mass spectrometry coupled with head space-solid phase microextraction.
abstract: An analytical method was developed for the identification and quantification of seven volatile n-nitrosamines (n-nitrosodimethylamine [NDMA], n-nitrosoethylmethylamine [NMEA], n-nitrosodiethylamine [NDEA], n-nitrosodipropylamine [NDPA], n-nitrosodibutylamine [NDBA], n-nitrosopiperidine [NPIP], and n-nitrosopyrrolidine [NPYR]) in water insoluble cream type cosmetics. It was found that the head space-solid phase microextraction (HS-SPME) was suitable for extraction, clean up, and pre-concentration of n-nitrosamines in the cream type samples so its optimal conditions were investigated. Identification and quantification of n-nitrosamines using single quadrupole gas chromatography/mass spectrometry (GC/MS) in chemical ionization (CI) mode were carried out with accurate mass measurements. Their accurate masses of protonated molecular ions were obtained within 10 mDa of the theoretical masses when sufficiently high signal was acquired from the unique calibration method using mass and isotope accuracy. For the method validation of quantification, spiking experiments were carried out to determine the linearity, recovery, and method detection limit (MDL) using three deuterated internal standards. The average recovery was 79% within 20% relative standard deviation (RSD) at the concentration of 50 ng/g. MDLs ranged from 0.46 ng/g to 36.54 ng/g, which was satisfactory for the directive limit of 50 ng/g proposed by the European Commission (EC). As a result, it was concluded that the method could be provided for the accurate mass screening, confirmation, and quantification of n-nitrosamines when applied to cosmetic inspection.
authors.affiliation: Department of Environmental Science and Engineering, Ewha Womans University, Seoul 120-750, South Korea.
authors.forename: Na Rae
authors.initials: NR
authors.lastname: Choi
authors.affiliation: Department of Environmental Science and Engineering, Ewha Womans University, Seoul 120-750, South Korea; Department of Chemical Engineering and Materials Science, Ewha Womans University, Seoul 120-750, South Korea.
authors.forename: Yong Pyo
authors.initials: YP
authors.lastname: Kim
authors.affiliation: Institute of Mine Reclamation Technology, Water and Soil Research and Development Team, Chungcheong 331-803, South Korea.
authors.forename: Won Hyun
authors.initials: WH
authors.lastname: Ji
authors.affiliation: Omics System Research Team, Western Seoul Center, Korea Basic Science Institute, Seoul 120-140, South Korea.
authors.forename: Geum-Sook
authors.initials: GS
authors.lastname: Hwang
authors.affiliation: Omics System Research Team, Western Seoul Center, Korea Basic Science Institute, Seoul 120-140, South Korea. Electronic address: ygahn@kbsi.re.kr.
authors.forename: Yun Gyong
authors.initials: YG
authors.lastname: Ahn
mesh_terms: D003358:Cosmetics / Q000032:analysis*; D004052:Diethylnitrosamine / Q000032:analysis; D004128:Dimethylnitrosamine / Q000031:analogs & derivatives / Q000032:analysis; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D009602:Nitrosamines / Q000032:analysis*; D052617:Solid Phase Microextraction / Q000379:methods*; D055549:Volatile Organic Compounds / Q000032:analysis
chemical_list: D003358:Cosmetics; D009602:Nitrosamines; D055549:Volatile Organic Compounds; C017510:methylethylnitrosamine; C013161:N-nitroso(di-n-propyl)amine; D004052:Diethylnitrosamine; C002743:N-nitrosopiperidine; C012279:dibutylnitrosamine; D004128:Dimethylnitrosamine
keywords: Accurate mass; Cosmetics; Gas chromatography/Chemical Ionization–Mass Spectrometry (GC/CI-MS); Head space-solid phase microextraction (HS-SPME); N-nitrosamines