Determination of synthetic musk compounds in indoor house dust by gas chromatography–ion trap mass spectrometry

Abstract

A new method for the simultaneous determination of 11 synthetic musks and one fragrance compound in house dust was developed. The nitro musks included musk ketone (MK, 4-tert-butyl-3,5-dinitro-2,6-dimethylacetophenone), musk xylene (MX, 1-tert-butyl-3,5-dimethyl-2,4,6-trinitrobenzene), musk ambrette (1-tert-butyl-2-methoxy-4-methyl-3,5-dinitrobenzene) and musk moskene (1,1,3,3,5-pentamethyl-4,6-dinitroindane). The polycyclic musk compounds were 1,3,4,6,7,8-hexahydro-4,6,6,7,8,8-hexamethylcyclopenta-(γ)-2-benzopyran (HHCB), 7-acetyl-1,1,3,4,4,6-hexamethyl-1,2,3,4-tetrahydronaphthalene (AHTN), 4-acetyl-1,1-dimethyl-6-tert-butylindane, 6-acetyl-1,1,2,3,3,5-hexamethylindane, 5-acetyl-1,1,2,6-tetramethyl-3-isopropylindane, 6,7-dihydro-1,1,2,3,3-pentamethyl-4(5H)-indanon. The one macrocyclic musk was 1,4-dioxacycloheptadecane-5,17-dione. The bicyclic hydrocarbon fragrance compound (1,2,3,4,5,6,7,8-octahydro-2,3,8,8-tetramethylnaphthalen-2yl)ethan-1-one (OTNE) and HHCB-lactone (4,6,6,7,8,8-hexamethyl-1H,3H,4H,6H,7H, 8H-indeno[5,6-c]pyran-1-one), a degradation product of HHCB, were also analysed. NIST SRM 2781 (domestic sludge) and SRM 2585 (organic contaminants in house dust) were analysed for these target compounds. The method was applied for the analysis of 49 paired samples collected using two vacuum sampling methods: a sample of fresh or "active" dust (FD) collected using a Pullman-Holt vacuum sampler, and a household dust (HD) sample taken from the participants' vacuum cleaners. Method detection limits and recoveries ranged from 12 to 48 ng/g and 54 to 117 %, respectively. AHTN, HHCB, OTNE and HHCB-lactone were detected in all samples, with median concentrations of 552, 676, 252 and 453 ng/g for FD samples, respectively; and 405, 992, 212 and 492 ng/g for HD samples, respectively. MX and MK were detected with high frequencies but with much lower concentrations. The two sampling methods produced comparable results for the target analytes. Widely scattered concentration levels were observed for target analytes from this set of 49 house dust samples, suggesting a wide variability in Canadian household exposure to synthetic musks.

Macrocyclic-, polycyclic-, and nitro musks in cosmetics, household commodities and indoor dusts collected from Japan: Implications for their human exposure

“…Several studies have reported the concentrations of synthetic musks in house dusts ( Table 2). The highest concentrations of HHCB, OTNE, and AHTN in dusts from Canada were 31,000, 5600, and 2400 ng/g, respectively (Kubwabo et al, 2012), which were greater than those in house dusts in Japan. The high concentrations of HHCB and AHTN were also found in house dusts from Germany at 11,400 and 3100 ng/g, respectively (Fromme et al, 2004).…”

“…This may be due to fast degradation of macrocyclic musks rather than other polycyclic and nitro musks (Suehiro, 1999). Kubwabo et al (2012) reported the occurrence of Musk T in Table 3 Estimated human exposure to Musk T and HHCB by using cosmetics and household commodoties in Japan.…”

“…Synthetic musks were also detected in house dusts from China, and HHCB and AHTN were dominant components, followed by nitro musks, such as musk xylene and musk ketone (Lu et al, 2011b, Liu et al, 2013. Kubwabo et al (2012) reported high concentrations of polycyclic musk, OTNE which marketed as 'Iso E Super' (CAS#: 54464-57-2), in house dusts collected from Canada. Further, it is noteworthy that macrocyclic musk, Musk T, was detected in dusts with high detection frequency of 43% (n ¼ 49).…”

Identifying Chemical Groups for Biomonitoring

“…At the same time, macrocyclic musks have come into greater use in Europe and in North America. Low levels of one macrocyclic musk were found in house dust samples from a Canadian study (Kubwabo et al 2012). Alicyclic musks appeared to be in use at the time we conducted our preliminary screen, but we found very little information on exposure or toxicity.…”

Concentrations and distribution of synthetic musks and siloxanes in sewage sludge of wastewater treatment plants in China

“…Both HHCB and AHTN have been featured as high production volume (HPV) chemicals by the US Environmental Protection Agency (EPA) and the 2007 OECD (Organization for Economic Co-operation and Development). More than 1000 tons/year of these two chemicals are produced or imported in at least one country/region among the OECD members (Kubwabo et al, 2012;Lu et al, 2011b). Due to their widespread use and low rates of degradation, SMs have been found not only in various environmental matrices (air, water and sediment, etc.…”