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TitleIntegrated Masters in Bioengineering Synthetic musks in personal care products
LanguageEnglish
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Page 1

Integrated Masters in Bioengineering





Synthetic musks in personal care products: method
development and exposure assessment




Master’s Thesis



of



Ana Carina de Carvalho Cunha


















Approved in public trials by Jury:



President: Professor Manuel José Vieira Simões

Examiner: Professor Valentina Maria Fernandes Domingues

FEUP Advisor: Professor Lúcia Maria da Silveira Santos

FEUP Co-Advisors: Professor Maria Arminda Costa Alves and Doctor Vera Maria Ferreira Cruz Homem





__________________________________________________________________





October 2012

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Synthetic musks in personal care products: method development and exposure assessment

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Table 9 – Retention times, quantification and identification ions of the targets

Compound Retention time (min) Target ions for GC–MS analysis

Cashmeran 20.60 191.2 + 163.2 + 135.2

Celestolide 30.04 229.4 + 173.2 + 244.3

Phantolide 31.42 229.4 + 187.2 + 171.6

Exaltolide 33.43 81.1 + 83.1 + 67.2 + 69.2

Musk ambrette 33.58 253.1 + 91.0 + 77.1

Galaxolide 34.06 243.3 + 213.3 + 128.3

Musk xylene


34.29 128.2 + 115.4 + 117.3

Tonalide 34.40 243.3 + 159.2 + 128.3

Musk moskene 34.91 263.2 + 128.4 + 115.2

Musk tibetene 36.05 251.2 + 115.4 + 128.4

Musk ketone 37.07 279.2 + 128.4 + 115.4

Ethylene brassylate 37.70 83.1 + 98.1 + 227.2 + 125.5



3.6 Quality assurance and control

Synthetic musks are present in a large number of PCPs and the analysis of these compounds asks

some discipline from the laboratory personnel in order to prevent contamination of samples. Cosmetics

were avoided whenever possible for labcoats, and detergents used in the laboratories as well as in the

personal use of the laboratory personnel. Room cleaning agents, such as floor polishers, window

cleaners, etc. must also be taken into account. Other sources of contamination are sunscreen protection

creams and lotions.

Procedural blanks were analyzed with every extraction batch. Trace levels of HHCB, DPMI and

exaltolide were detected in procedural blanks. Blank values were subtracted for all of the

concentrations reported. Limits of detection (LODs) and limits of quantification (LOQs) were calculated

as the concentration giving a signal-to-noise ratio of three (S/N = 3) and of 10 (S/N = 10), respectively.

Recovery tests were performed by spiking with a standard mixture containing the synthetic musks into

selected products (one of each category) at three levels (100, 200 and 400 ng).

In this GC-MS methodology, an external standard calibration curve was used for musks

quantification. In order to assess the response stability over time, a 400 μg.L
-1

standard control was

injected daily.

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Synthetic musks in personal care products: method development and exposure assessment

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3.7 Waste treatment

The waste generated in this work consisted in organic solutions containing acetonitrile and traces

of musks and mixtures of different sorbents (MgSO4, NaCH3COO, PSA and C18) contaminated with musks.

All these residues were collected in closed containers, properly labelled, and they were stored protected

from light and from ignition sources for further treatment by the Environmental Management System of

FEUP - EcoFEUP.

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Synthetic musks in personal care products: method development and exposure assessment

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Table A 23 - Skin Moisturisers (n = 12) mean, minimum and maximum concentrations (µg/g), n, and frequency of occurrence (%)

Body Moisturisers Facial creams

Compound BL 1 BL 2 BL 3 BL 4 BL 5 BL 6 BL 7 BL 8 BL 9 FC 1 FC 2 FC 3 Mean n Frequency Min. Max.

Cashmeran 3.430 0.168 0.930 0.397 7.519 1.712 0.849 3.898 0.958 2.133 0.451 -- 2.040 11 92 0.168 7.519

Celestolide 0.328 -- -- -- -- -- -- -- -- 0.093 -- -- 0.210 2 17 0.093 0.328

Phantolide -- -- -- 0.054 -- -- -- -- -- 0.301 -- -- 0.177 2 17 0.054 0.301

Exaltolide -- -- 11.681 7.266 8.369 19.917 14.329 5.806 58.303 3.741 11.907 4.897 14.621 10 83 3.741 58.303

M. Ambrette -- -- -- -- -- -- -- -- -- -- -- -- -- 0 0 -- --

Galaxolide 882.340 -- 0.698 58.170 0.960 0.888 1.011 -- 0.052 56.900 0.586 -- 111.291 9 75 0.052 882.340

M. Xylene -- -- -- -- -- -- -- -- -- -- -- -- -- 0 0 -- --

Tonalide 203.660 5.308 -- -- -- -- -- -- -- 5.026 -- -- 71.331 3 25 5.026 203.660

M. Moskene -- -- -- -- -- -- -- -- -- -- -- -- -- 0 0 -- --

M. Tibetene -- -- -- -- -- -- -- -- -- -- -- -- -- 0 0 -- --

M. Ketone -- -- -- -- -- -- -- -- -- -- -- -- -- 0 0 -- --

Total 199.670



Table A 24 - Body and hair washes (n = 17) mean, minimum and maximum concentrations (µg/g), n, and frequency of occurrence (%)

Liquid soaps Shampoos Shower gels

Compound LS 1 LS 2 LS 3 SH 1 SH 2 SH 3 SH 4 SH 5 SH 6 SG 1 SG 2 SG 3 SG 4 SG 5 SG 6 SG 7 SG8 Mean n Frequency Min. Max.

Cashmeran 5.142 0.916 1.179 0.180 7.385 -- 0.764 1.713 0.041 6.995 8.697 6.261 -- 2.551 2.126 -- 2.364 3.308 14 82 0.041 8.697

Celestolide -- 0.124 -- -- 0.047 -- 0.217 0.139 -- -- -- -- -- -- -- -- -- 0.132 4 24 0.047 0.217

Phantolide -- 0.021 0.008 -- 0.008 -- 0.033 0.019 -- -- 0.280 0.032 -- -- -- -- -- 0.057 7 41 0.008 0.280

Exaltolide 0.254 6.256 4.061 -- 1.552 1.502 39.841 29.062 2.824 -- 7.258 -- 36.864 1.112 -- -- 0.198 10.899 12 71 0.198 39.841

M. Ambrette -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- 0 0 -- --

Galaxolide 0.018 134.185 0.014 0.293 192.381 0.015 451.652 410.383 0.004 0.032 0.034 730.142 0.025 0.006 0.144 0.072 0.004 112.906 17 100 0.004 730.142

M. Xylene -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- 0 0 -- --

Tonalide -- 1.486 -- -- 1.166 -- 1.668 2.567 -- -- -- 5.410 -- -- -- -- -- 2.460 5 29 1.166 5.410

M. Moskene -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- 0 0 -- --

M. Tibetene -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- 0 0 -- --

M. Ketone -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- 0 0 -- --

Total 129.761

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Synthetic musks in personal care products: method development and exposure assessment

96

Appendix 3 Exposure assessment



Mean and total concentrations of the studied synthetic musks, necessary to calculate the

exposure assessment to skin moisturisers, toothpastes, deodorants, toilet soaps, body and hair washes

are presented in Table A 25.




Table A 25 – Mean and total concentrations (µg/g) of musks in different categories of personal care products

Body lotions Facial creams Toothpastes Deodorants Toilet soaps Liquid soaps Shampoos Shower gels

Cashmeran 2.207 1.292 -- 6.508 2.790 2.412 2.016 4.832

Celestolide 0.328 0.093 -- 0.134 0.086 0.124 0.134 --

Phantolide 0.054 0.301 -- 0.028 -- 0.014 0.020 0.156

Exaltolide 17.953 6.848 -- 22.423 5.683 3.524 14.956 11.358

M. Ambrette -- -- -- -- -- -- -- --

Galaxolide 134.875 28.743 0.00329081 66.903 17.812 44.739 175.788 91.307

M. Xylene -- -- -- -- -- -- -- --

Tonalide 104.484 5.026 3.684 0.169 1.486 1.800 5.410

M. Moskene -- -- -- -- -- -- -- --

M. Tibetene -- -- -- -- -- -- -- --

M. Ketone -- -- -- -- -- -- -- --

Ethylene Brassylate -- -- -- -- 0.736 -- -- --

Total 259.900 42.302 0.003 99.6819 27.277 52.300 194.716 113.063

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