Development and validation of a gas chromatography–mass spectrometry method for determination of 30 fragrance substances in cosmetic products

Abstract

A QuEChERS sample preparation, for a broad-range of cosmetic products, followed by gas chromatography-mass spectrometry analysis was developed for the simultaneous determination of 30 fragrance substances. The sample preparation step was optimized for different leave-on and rinse-off cosmetic products. A small amount of sample (1 g) was extracted with acetonitrile, the extract was subject to a rapid QuEChERS clean up followed by centrifugation and the organic layer was collected for gas chromatography-mass spectrometry analysis. The gas chromatography-mass spectrometry method was developed on a mid-polarity GC capillary column (30 m, ZB-35HT) to obtain maximum separation of the targeted compounds in less than 60 min. Using this method, the method limit of detection and the method limit of quantitation for the 30 fragrance substances, were determined as 0.1-1.2 µg/g and 0.33-4.0 µg/g, respectively. For most of the fragrance substances, the spike recovery values were 80-120% with a relative standard deviation < 10% for all fragrance substances in three tested matrices (shampoo, lotion, and deodorant). This method was applied to evaluate 42 commercial cosmetic products purchased from nine different countries. Of the 30 leave-on products, 18 products measured at least one fragrance above 10 µg/g and 5 of the 12 rinse-off products measured at least one fragrance above 100 µg/g. According to the European regulation (EC, No 1223/2009, ANNEX III), 24 of these fragrance substances are subject to specific labeling requirements if any individual concentration exceeds 10 µg/g for leave-on and 100 µg/g for rinse-off products. Our results show that this method can be applied to various cosmetic products for determination of fragrance substances designated "allergens" in the European Union.

Mass-Spectrometry-Based Research of Cosmetic Ingredients

“…GC-MS is the most popular technique for fragrance analysis since they usually have low boiling points. Currently, GC is extensively used for sample infusion in EI-MS and has been greatly applied for the determination of allergens [ 28 , 31 , 98 , 107 , 144 , 145 , 146 , 147 , 148 , 149 , 150 , 151 , 152 , 153 , 154 , 155 , 156 , 157 , 158 , 159 , 160 , 161 , 162 , 163 , 164 , 165 , 166 ] and other risky components in cosmetic analysis ( Table A1 ). In addition to EI, other ionization techniques like chemical ionization (CI) and photoionization (PI) are employed for GC-MS investigations in this field.…”

“… GC-MS Simultaneous determination of 30 fragrances (including 24 listed allergens)—18 leave-on products contained at least one fragrance substance > 10 µg/g and 5 of the 12 rinse-off products contained at least one fragrance substance > 100 µg/g. [ 166 ] 2 A total of 166 leave-on cosmetic products purchased within three years and stored at room temperature. GC-MS and GC-MS/MS The method was tested in order to identify the presence of 24 regulated allergens and 21 prohibited substances in the cosmetic products: 2–17 allergens were identified per sample, and only safrole (of the prohibited substances) was present in a concentration > LOQ in 12 out of 166 tested samples.…”

Electrochemical sensing platform with gold nanoparticles capped by PDDA for benzyl alcohol determination

“…This work presents the first AuNP-based electrochemical sensor for the determination of benzyl alcohol, a preservative widely added to cosmetics, but the maximum allowed concentration in these products is regulated since this compound is considered a chemical sensitizer [ 15 , 16 ]. Benzyl alcohol is usually determined by HPLC methods coupled to diode-array (DAD) or mass spectrometer (MS) detectors [ 17 , 18 ]. Electrochemical methods are an alternative to the chromatographic ones since they benefit from good properties such as low sample and reagents consumption, real-time analysis and good sensitivity in the measurements.…”