Determination of nine nitrobenzene compounds in cosmetics by ultra performance liquid chromatography quadrupole-time-of-flight mass spectrometry
An ultra performance liquid chromatography-quadrupole-time-flight mass spectrometric method was developed for the simultaneous screening and determination of 9 nitrobenzene compounds,including nitrobenzene(NB),3,4-dinitrotoluene(3,4-DNT),2,3-dinitrotoluene(2,3-DNT),2,4-dinitrotoluene(2,4-DNT),2,6-dinitrotoluene(2,6-DNT),2,5-dinitrotoluene(2,5-DNT),3,5-dinitrotoluene(3,5-DNT),2-nitrotoluene(2-NT)and 1-chloro-4-nitrobenzene(ChNB)in cosmetics.Samples were extracted with ethyl acetate,and the extracts were further hydrogenated using 5％Pd/C catalyst.The target analytes were separated on a Poroshell 120 EC-C18 chromatographic column(100 mm × 4.6 mm,2.7 μm).Gradient elution was carried out with 0.1％(V/V)formic acid aqueous solution and acetonitrile as the mobile phases.The eluent from the column was further detected using Q-tof MS with information dependent acquisition(Auto MS/MS)mode for MS data acquisition.A database,containing retention time,precise mass of parent ion,isotope abundance ratio and precise mass of fragment ion,was established for screening and confirming the nitrobenzene compounds.The quantitation analysis was carried out by extracting peak area with precise mass.Under optimal conditions,the analytes show good linear relationship within the range,with the correlation coefficient(r)not less than 0.999.The limits of detection are in the range of 0.01-0.3 mg/kg,and the limits of quantification are in the range of 0.04-2.0 mg/kg.Samples,such as cream,lotion,powder and lip balm,are fortified at three levels.The average spiked recoveries range from 85.2％to 113％,with the relative standard deviations(RSDs)ranging from 0.23％to 3.61％.The optimized method is accurate,sensitive,specific and suitable for the detection and screening of nitrobenzene compounds in cosmetics.
ultra performance liquid chromatographyquadrupole-time-flight mass spectrometrynitrobenzene compoundscosmetics
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