Study Of The Analysis Of Two Limited Nitro-musk Compounds And Four Inhibited Nitroso-compounds In Cosmetics

Two nitro-musk compounds musk xylene and musk ketone are limited compounds incosmetics, and four nitroso-compounds (4-nitrosophenol/1-methyl-3-nitro-1-nitrosoguanidine/isobutyl nitrite and amyl nitrite are inhibited compounds in cosmetics. After studying thecharacters of these substances, this paper developed the chromatography analytical methodsof the two kinds of material. Main content as follows:(1) A gas chromatography–flamionization detection (GC-FID) method was used for the determination of two nitro-muskcompounds musk xylene and musk ketone simultaneously which are limited in cosmetics. Thecosmetic sample was dissolved in the organic solvent and extracted under ultrasonication. Theextraction was dehydrated with anhydrous sodium sulfate and filtrated using organic dialyzerwith0.45μm aperture. The analysis was carried out by FID after the chromatographicseparation on HP-INNOWAX capillary column. Musk xylene and musk ketone wereanalyzed qualitatively based on their retention time. The quantitative analysis was carried outby external standard method. The experiment’s result shows that the two compounds bothhave good linearity in the concentration between10μg/ml~500μg/ml. The detection limit ofmusk xylene and musk ketone was5μg/g and3.5μg/g, and the average recoveries were92.23%~105.6%and93.19%~105.1%, with the RSD both less than5%.(2) Studied thecharacters of four inhibited nitroso-compounds, developed the analytical methods of thesesubstances.①A high performance liquid chromatography–(DAD) method was used for thedetermination of two inhibited nitroso-compounds (4-nitrosophenol and1-methyl-3-nitro-1-nitrosoguanidine). The cosmetic sample was dissolved in the organic solvent and extractedunder ultrasonication. The extracts were analyzed by HPLC using a C18reversed-phasecolumn, DAD detector was used for canning with the detection wavelength at284nm. Underthe optimal conditions,4-nitrosophenol and1-methyl-3-nitro-1-nitrosoguanidine wasanalyzed qualitatively based on its retention time and ultraviolet absorption spectrum. Thequantitative analysis was carried out by external standard method. The calibration curvesshowed good linearity between0.5μg/ml and10μg/ml. The detection limit of4-nitrosophenol and1-methyl-3-nitro-1-nitrosoguanidine was20ng/g, and the averagerecoveries were94.14%~102.8%and96.3%~104.1%, with the RSD both less than3.5%.②Agas chromatography–flam ionization detection (GC-FID) method was used for the determination of two inhibited nitrous acid esters isobutyl nitrite and amyl nitrite in cosmeticssimultaneously.2%sodium sulfite solution was added in the sample of cosmetics and theextraction solvent was acetone, and then the extraction was further dehydrated withanhydrous sodium sulfate and filtrated using organic dialyzer with0.45μm aperture. Thefiltrate was determined by gas chromatography with flame ionization detection (GC-FID).The experiment’s result shows that the two compounds both have good linearity in theconcentration between10μg/ml~1000μg/ml. The detection limit of isobutyl nitrite and amylnitrite was4μg/g and2μg/g, and the average recoveries were87.03%~98.83%and86.80%~96.90%, with the RSD less than6%and5%respectively.