New analytical method for the determination of musks in personal care products by Quick, Easy, Cheap, Effective, Rugged, and Safe extraction followed by GC–MS

Abstract

Synthetic musks are organic compounds used as fragrance additives and fixative compounds in a diversity of personal care products. A new method based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction followed by GC-MS for the analysis of 12 musks in personal care products was developed and validated. Some experimental parameters, such as total QuEChERS mass, sample mass/solvent volume ratio, type of extraction solvent, as well as salts and sorbents amount were investigated and optimized. The final method involves the musks extraction using acetonitrile, followed by the addition of anhydrous magnesium sulphate and sodium acetate. The clean-up step was performed using dispersive SPE with primary and secondary amine and octadecyl-silica sorbents. This extraction procedure is fast (about 10 min) when compared to other traditional approaches. The method was robust for the matrices studied and shows a high precision (%RSD < 15%) and accuracy (average recovery of 85%), allowing the detection of musks in minimum concentrations between 0.01 ng/g (galaxolide) and 15.80 ng/g (musk xylene). The developed method was applied to the analysis of 12 samples, which revealed musks concentrations ranging from 2 ng/g (toothpaste) to 882,340 ng/g (perfumed body lotion).

Using air, soil and vegetation to assess the environmental behaviour of siloxanes

“…The eluate was then reduced to approximately 1 mL by rotary evaporation, transferred to glass vials, evaporated to near dryness by N2 and redissolved in 150 μL of Hex. For soils and pine needles, the QuEChERS technology employed was based in a previous setup developed for the determination of synthetic musk fragrances in personal care products (Homem et al 2013). Soils or pine needles (2.5 g) spiked with 15 ng g −1 of M4Q and placed into 50-mL polypropylene conical bottom centrifuge tubes were extracted for 15 min in an ultrasonic bath (420 W) with 10 mL of DCM/Hex 1:1.…”

“…In this study, it was decided to use a more environment-friendly approach employing the quick, easy, cheap, effective, rugged and safe (QuEChERS) method for the soils and pine needles, following previous work done in our group to extract musks from personal care products (Homem et al 2013).…”

Scented traces – Dermal exposure of synthetic musk fragrances in personal care products and environmental input assessment

“…Details of the extraction have been described elsewhere (Homem et al, 2013). Briefly, 3 mL of acetonitrile was added to 500 mg of each sample and the mixture were vortexed and sonicated during 3 min and 10 min, respectively.…”

“…Acquisition was made in selected ion storage (SIS) mode and synthetic musks were identified and quantified using retention time and up to three ions with the Varian MS workstation v. 6.9.3 software. The ions monitored for individual compounds have been previously reported (Homem et al, 2013).…”

“…Although several studies have been conducted to determine synthetic musks in environmental and human body compartments, few have focused on the determination of these compounds in PCPs. In fact, most studies present the development of new analytical methodologies to determine synthetic musks in PCPs (Dong et al, 2014;Correia et al, 2013;Homem et al, 2013;Llompart et al, 2013;Sanchez-Prado et al, 2011), but very few have assessed human exposure to these compounds, analysing a large sample pool (more than 100 samples from different categories of products) (Lu et al, 2011).…”