Evaluation of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) in pure mineral hydrocarbon-based cosmetics and cosmetic raw materials using ¹H NMR spectroscopy

Mineral hydrocarbons consist of two fractions, mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH). MOAH is a potential public health hazard because it may include carcinogenic polycyclic compounds. In the present study, 400 MHz nuclear magnetic resonance (NMR) spectroscopy was introduced, in the context of official controls, to measure MOSH and MOAH in raw materials or pure mineral hydrocarbon final products (cosmetics and medicinal products). Quantitative determination (qNMR) has been established using the ERETIC methodology (electronic reference to access in vivo concentrations) based on the PULCON principle (pulse length based concentration determination). Various mineral hydrocarbons (e.g., white oils, paraffins or petroleum jelly) were dissolved in deuterated chloroform. The ERETIC factor was established using a quantification reference sample containing ethylbenzene and tetrachloronitrobenzene. The following spectral regions were integrated: MOSH δ 3.0 – 0.2 ppm and MOAH δ 9.2 - 6.5, excluding solvent signals. Validation showed a sufficient precision of the method with a coefficient of variation <6% and a limit of detection <0.1 g/100 g. The applicability of the method was proven by analysing 27 authentic samples with MOSH and MOAH contents in the range of 90-109 g/100 g and 0.02-1.10 g/100 g, respectively. It is important to distinguish this new NMR-approach from the hyphenated liquid chromatography-gas chromatography methodology previously used to characterize MOSH/MOAH amounts in cosmetic products. For mineral hydrocarbon raw materials or pure mineral hydrocarbon-based cosmetic products, NMR delivers higher specificity without any sample preparation besides dilution. Our sample survey shows that previous methods may have overestimated the MOAH amount in mineral oil products and opens new paths to characterize this fraction. Therefore, the developed method can be applied for routine monitoring of consumer products aiming to minimize public health risks

Quantification of Mineral Oil Aromatic Hydrocarbons (MOAH) in Anhydrous Cosmetics Using 1 H NMR

In cosmetic products, hydrocarbons from mineral oil origin are used as ingredients in a wide variety of consistency, from liquid oil to solid wax. Refined mineral oil hydrocarbons consist of MOSH (mineral oil saturated hydrocarbons) and a low proportion of MOAH (mineral oil aromatic hydrocarbons). MOSH and MOAH comprise a variety of chemically similar single substances with straight or branched chains. In the context of precautionary consumer protection, it is crucial to determine hydrocarbons from mineral oil origin of inferior quality quickly and efficiently. This publication presents a rapid method for quantifying MOAH by proton nuclear magnetic resonance spectroscopy (¹H qNMR) in anhydrous cosmetics such as lipstick, lip gloss, and lip balm. A sample clean-up using solid-phase extraction (SPE) was developed for the complete removal of interfering aromatic substances to improve the robustness of the method for analysing compounded cosmetics. In preliminary trials using silica gel thin-layer chromatography, the retention behaviour of 21 common aromatic compounds was tested in eluents with different solvent strength including EtOAc, MeOH, cyclohexane, and dichloromethane. Based on these results, the SPE sample cleanup with silica gel and cyclohexane as an eluent was suggested as best suitable for the purpose. The SPE cleanup was successfully achieved for all tested potentially interfering aromatic cosmetic ingredients except for butylated hydroxytoluene. The recovery for lipophilic cosmetics is more than 80% based on naphthalene as calculation equivalent. Furthermore, a specific sample preparation for the examination of lipsticks was implemented. The SPE cleanup was validated, and the robustness of the method was tested on 57 samples from the retail trade. The ¹H qNMR method is a good complement to the LC-GC-FID method, which is predominantly used for the determination of MOSH and MOAH. Chromatographic problems such as migration of MOSH into the MOAH fraction during LC-GC-FID can be avoided

Evaluation of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) in pure mineral hydrocarbon-based cosmetics and cosmetic raw materials using 1H NMR spectroscopy [version 2; referees: 3 approved]

Mineral hydrocarbons consist of two fractions, mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH). MOAH is a potential public health hazard because it may include carcinogenic polycyclic compounds. In the present study, 400 MHz nuclear magnetic resonance (NMR) spectroscopy was introduced, in the context of official controls, to measure MOSH and MOAH in raw materials or pure mineral hydrocarbon final products (cosmetics and medicinal products). Quantitative determination (qNMR) has been established using the ERETIC methodology (electronic reference to access in vivo concentrations) based on the PULCON principle (pulse length based concentration determination). Various mineral hydrocarbons (e.g., white oils, paraffins or petroleum jelly) were dissolved in deuterated chloroform. The ERETIC factor was established using a quantification reference sample containing ethylbenzene and tetrachloronitrobenzene. The following spectral regions were integrated: MOSH δ 3.0 – 0.2 ppm and MOAH δ 9.2 - 6.5, excluding solvent signals. Validation showed a sufficient precision of the method with a coefficient of variation <6% and a limit of detection <0.1 g/100 g. The applicability of the method was proven by analysing 27 authentic samples with MOSH and MOAH contents in the range of 90-109 g/100 g and 0.02-1.10 g/100 g, respectively. It is important to distinguish this new NMR-approach from the hyphenated liquid chromatography-gas chromatography methodology previously used to characterize MOSH/MOAH amounts in cosmetic products. For mineral hydrocarbon raw materials or pure mineral hydrocarbon-based cosmetic products, NMR delivers higher specificity without any sample preparation besides dilution. Our sample survey shows that previous methods may have overestimated the MOAH amount in mineral oil products and opens new paths to characterize this fraction. Therefore, the developed method can be applied for routine monitoring of consumer products aiming to minimize public health risks

Evaluation of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) in pure mineral hydrocarbon-based cosmetics and cosmetic raw materials using 1H NMR spectroscopy [version 1; referees: 2 approved, 1 approved with reservations]

Mineral hydrocarbons consist of two fractions, mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH). MOAH is a potential public health hazard because it may include carcinogenic polycyclic compounds. In the present study, 400 MHz nuclear magnetic resonance (NMR) spectroscopy was introduced, in the context of official controls, to measure MOSH and MOAH in raw materials or pure mineral hydrocarbon final products (cosmetics and medicinal products). Quantitative determination (qNMR) has been established using the ERETIC methodology (electronic reference to access in vivo concentrations) based on the PULCON principle (pulse length based concentration determination). Various mineral hydrocarbons (e.g., white oils, paraffins or petroleum jelly) were dissolved in deuterated chloroform. The ERETIC factor was established using a quantification reference sample containing ethylbenzene and tetrachloronitrobenzene. The following spectral regions were integrated: MOSH δ 3.0 – 0.2 ppm and MOAH δ 9.2 - 6.5, excluding solvent signals. Validation showed a sufficient precision of the method with a coefficient of variation <6% and a limit of detection <0.1 g/100 g. The applicability of the method was proven by analysing 27 authentic samples with MOSH and MOAH contents in the range of 90-109 g/100 g and 0.02-1.10 g/100 g, respectively. It is important to distinguish this new NMR-approach from the hyphenated liquid chromatography-gas chromatography methodology previously used to characterize MOSH/MOAH amounts in cosmetic products. For mineral hydrocarbon raw materials or pure mineral hydrocarbon-based cosmetic products, NMR delivers higher specificity without any sample preparation besides dilution. Our sample survey shows that previous methods may have overestimated the MOAH amount in mineral oil products and opens new paths to characterize this fraction. Therefore, the developed method can be applied for routine monitoring of consumer products aiming to minimize public health risks

Gas chromatographic analysis of volatile hydrocarbons to detect irradiated chicken, pork and beef - an intercomparison study A report in English and German

This report provides a detailed description of an inter-laboratory study to detect irradiation treatment of chicken carcasses, pork and beef using a method suitable for routine application. The 17 participating laboratories determined the quantity of four different radiation-induced hydrocarbons (1-tetradecene, pentadecane, 1,7-hexadecadiene, 8-heptadecene) in coded samples approx. 3 and 6 months after irradiation. The quantities detected were used to identify the samples as irradiated or non-irradiated. The samples of each type of meat to be examined had been supplied by two different producers. The dose range that was tested (approx. 0.6 to 7.5 kGy) included commercially used doses (approx. 1 to 5 kGy). The method employed enable 98.3% of a total of 864 samples to be correctly identified as irradiated or non-irradiated. This result is remarkable: Although the marker concentrations in the various samples showed a clear dose dependency, the variation was quite marked. The high rate of correct identifications could be achieved by defining a sample only as irradiated if certain quantities of at least 3 of the radiolytic products to be determined had been found. A similar identification rate was achieved if quantification of markers was omitted to identify a sample only as irradiated when all the expected radiolysis products could be clearly detected. For all three types of meat, no significant differences in marker yields could be shown for the products of the respective two producers. Also, in none of the types of meat, any significant difference could be revealed for the quantiatitive results achieved three and six months after irradiation. These results show that irradiation of chicken carcasses, pork and beef in the commerically used dose range can be clearly detected throughout the entire period in which products are normally stored and that the method described is suitable for routine analyses in food control laboratories. (orig.)Available from TIB Hannover: RR 1068(1993,1) / FIZ - Fachinformationszzentrum Karlsruhe / TIB - Technische InformationsbibliothekSIGLEDEGerman