顶空固相微萃取-气相色谱-质谱联用测定香水中5种合成麝香

A method for headspace solid-phase microextraction(HS-SPME),followed by gas chromatography-mass spectrometry(GC-MS) analysis was established for the determination of five commonly used synthetic musks in perfume.Two polycyclic musks(celestolide and tonalide) and three nitro musks(musk ambrette,musk xylene and musk ketone) were used as analytes in the optimization of the analytical method.Six parameters,such as the extraction temperature,equilibrium time,extraction time,desorption time,injector temperature and solution of salting out,were optimized by exposing the 65 μm polydimethylsiloxane-divinylbenzene(PDMS-DVB) fiber to the headspace of magnetically stirred(600 r/min) sample.According to the results of the optimization experiments,the following conclusion can be drawn: The water-diluted sample in a 10 mL headspace-vial was efficiently extracted for 20 min after the system was equilibrated for 3 min at 60 ℃.After extraction,the fiber was immediately inserted into the GC injector and desorbed at 250 ℃ for 3 min.The spiked recoveries were in the range of 82.0%-103.3% and the relative standard deviations(RSDs) were between 1.8% and 9.4%.Meanwhile,the limits of detection(LODs) ranged from 0.6 ng/g to 2.1 ng/g.This method is characterized by rapidity,high sensitivity,good linearity and repeatability for all the target compounds.It is applicable to the analysis of synthetic musks in perfumes.