A rapid and sensitive gas chromatography-mass spectrometry method for the quality control of perfumes: simultaneous determination of phthalates

Abstract

A rapid and sensitive analytical gas chromatography-mass spectrometry (GC-MS) method for perfume analysis to determine the phthalates banned by the European Union Regulation on cosmetic samples is presented. This method has been tested in commercial alcoholic perfume samples for the determination of the following seven phthalates: dibutyl phthalate, bis(2-ethylhexyl) phthalate, bis(2-methoxyethyl) phthalate, npentyl-isopentylphthalate, di-n-pentyl phthalate, diisopentylphthalate and benzyl butyl phthalate.Sample evaporation and redissolution in ethanol is carried out before GC-MS analysis, with no dilution of the sample.External and standard addition calibration are compared to detect possible matrix effects. External calibration could provide good results in some cases but standard addition calibration is recommended as matrix effects are observed in many cases in the determination of the target phthalates.The accuracy of the method has been proven by the analysis of quality control samples prepared from commercial free phthalates perfumes after spiking with known concentrations of the analytes. Accurate results were obtained with limits of detection in the ng mL -1 range and good repeatability (relative standard deviations lower than 6 %). The method was satisfactorily applied to the analysis of commercial perfume samples, and the results revealed considerable amounts of dibutyl phthalate and bis(2-ethylhexyl) phthalate in some of the analyzed samples.

Development and validation of a dispersive liquid–liquid microextraction method for the determination of phthalate esters in perfumes using gas chromatography-mass spectrometry

“…Moreover, a high dilution is usually required when analyzing perfume samples using GC-MS to avoid the introduction of high water content into the GC column. 32 Therefore, in this work, DLLME method was developed to preconcentrate and determine PEs at sub ppm levels.…”

“…31,32 Due to the high concentration of some of the target analytes (especially DEP), all real samples were diluted by a factor of 5 to 50 with deionized water to achieve the proper quantitation of all analytes. Moreover, a high dilution is usually required when analyzing perfume samples using GC-MS to avoid the introduction of high water content into the GC column.…”

“…9,18,19,[28][29][30][31] Several studies have reported the presence PEs in perfumes in wide concentration ranges from sub ppm to high percentage. 31,32 Therefore a preconcentration step is usually required in order to determine PEs at sub ppm levels.…”

“…Different sample preparation techniques such as direct dilution, 19 vortex extraction, 28 ultrasonic extraction treatment using organic solvents 18,22,29 or solid phase microextraction 31 have been used for extracting PEs.…”

“…9,[14][15][16][17][18][19][20][21][22][23][24][25][26][27] The most commonly used technique for the determination of PEs in perfumes is gas chromatography -mass spectrometry (GC-MS) e.g. 9,18,19,[28][29][30][31] Several studies have reported the presence PEs in perfumes in wide concentration ranges from sub ppm to high percentage. 31,32 Therefore a preconcentration step is usually required in order to determine PEs at sub ppm levels.…”