| Front page | | Contents | | Previous | | Next |

Survey of lip care products with fragrance and flavour

6 Analyses

• 6.1 Fragrances
• 6.2 Analytical methods
  • 6.2.1 Methyl eugenol
  • 6.2.2 Fragrances
• 6.3 Results
  • 6.3.1 Methyl eugenol
  • 6.3.2 Fragrances
• 6.4 Summary of analytical results
• 6.5 Selection of substances for health assessment

6.1 Fragrances

Emphasis was placed on including both expensive and low-priced product as well as products for children and adults alike when selecting the products for analysis of the 26 fragrances. Twenty products were selected for analyses of the 26 fragrances. Furthermore, three products, which according to their declaration of contents contain rose oil, were selected for analysis of methyl eugenol. Based on the marketing of the products, the three rose oil-containing products are all assessed to be for adults. Of the 20 selected products for analysis, 3 products are assessed to appeal to adults, 7 to the young and 10 to children.

The following products were selected for analysis:

Two products with strawberry fragrance, 2 with orange fragrance, 2 with raspberry fragrance, 2 with melon fragrance, 1 with banana fragrance, 1 with pineapple fragrance, 1 with papaya fragrance, and 1 with "tropical" fragrance listed on the packaging. The remaining 8 products selected for analysis did not have a defined fragrance (cf. 4.1.3) listed on the packaging or in the declaration of contents. However, some of these products had a characteristic fragrance such as peppermint or orange while others merely had a sweet or flowerlike fragrance.

6.2 Analytical methods

6.2.1 Methyl eugenol

A part sample of the product is extracted with dichloromethane for two hours on a shaker followed by one-hour ultrasound treatment. A part sample of the extract is taken and analysed directly at combined gas chromatography and mass spectrometry (GC/MS). The content is calculated quantitatively.

Uncertainty is 10-15% RSD. The analyses are performed as true double determinations. The limit of detection is 10 mg/kg.

6.2.2 Fragrances

A part sample of the products is taken and extracted with water and tert-butyl methyl ether by means of shaking, heating, cooling, and standing during a period of approximately 16 hours. A part sample of the extract is taken and analysed directly at combined gas chromatography and mass spectrometry (GC/MS). The analyses are performed as true double determinations. The limit of detection is 1-10 mg/kg and the uncertainty is 10-15% RSD.

6.3 Results

6.3.1 Methyl eugenol

Three products were analysed for methyl eugenol and the result of the analyses are given in table 6.1. The table contains two results due to double determination (A and B). The unit is mg/kg and the limit of detection is 10 mg/kg.

Table 6.1 The results of the analysis for methyl eugenol. The results are given in mg/kg.

<: means less than the stated limit of detection

Maximum allowed amount in this type of cosmetic products are 2 mg/kg (0,0002 %). The results shows that product 80 og product 93 contains illegal amounts of methyl eugenol. These offences are dealt with by the Chemical Inspection Service. The producers have subsequent changes the content of the product so the present products now are legal.

6.3.2 Fragrances

All 20 products were analysed for 26 fragrances. Only one product showed no content of any of the 26 components. The total content of all 26 fragrances are given at the bottom of the table. The total content varies from 6 to 26,000 mg/kg.

The two highest contents were determined in amounts ranging from 15,000 to 26,000 mg/kg corresponding to 1.5-2.6 weight%. Both accounts were due to an extremely high content of D-limonene compared to the other components.

A summary of the results of the analyses can be seen in table 6.2.

Table 6.2. Analytical results of the fragrances. The unit is mg/kg. The result states the average of the double determinations.

Click here to see table 6.2

6.4 Summary of analytical results

Eleven of the 26 fragrances were not found in any of the 20 analysed lip care products. Total occurrence of fragrances in the 20 analysed lip care products is 84, i.e. an average of 4.2 fragrances per product. One or more of the tested fragrances occurred in 19 of the 20 analysed products.

The occurrence of fragrances were distributed like this:

aα-Isomethylionon, coumarin and cinnamal were found in 1 product; isoeugenol, farnesol and benzyl salicylat was found in 2 products; benzyl cinnamat was found in 3 products; citral in 4 products; citronellol in 5 products; eugenol in 6 products; benzyl benzoate and geraniol in 8 products; benzyl alcohol in 10 products; linalool in 12 products, and d-limonen in 19 products.

Anisyl alcohol, amyl cinnamal, amylcinnamal alcohol, cinnamyl alcohol, hexylcinnamaldehyd, hydroxycitronellal, lillial, lyral, methyl hoptin carbonal, oakmoss and treemoss were not found in any of the analysed products.

Table 6.3 shows the number of fragrances found in the products, including the target group of the product.

Table 6.3. Number of fragrances found per product and product target group.

A large spread of concentrations in the products is seen for both single substances and the total content of the 26 fragrances. It appears that a high content of D-limonen is also the cause of a high total content of perfume.

Total perfume content in percentage by weight was 0% in one product; between 0 and 0.1% in 11 products; between 0.1 and 1% in 6 products; and > 1% (1.55 and 2.45 percentage by weight) in 2 products.

The three products selected for analysis of the 26 fragrances and analysis of methyl eugenol were the only three selected products with adults as the target group. Of the remaining 17 products, 10 products are estimated to be products for children and 7 products to be products for the young. The three products were estimated to be products for adults based on their price, product appearance and placing of the product in the shops. These products turned out to have a total perfume content of 15,500, 1,400 and 420 mg/kg respectively made of 5, 9 and 10 different fragrances. Consequently, the "adult products" represent the two products in the analysis in which the largest different number of the 26 allergenic fragrances was identified as well as the second highest total perfume content measured. The remaining content of 1,400 and 420 mg/kg is reasonably in line with the products for children and the young. In addition, plant extracts are typical ingredients in "adult products".

Table 6.4 sums up the analytical results with the occurrence in number of products, minimum and maximum measured values and the maximum value as the fragrance's percentage by weight in the product.

Table 6.4. Summary of analytical results.

* Except for D-limonen, the weight percentage is given with 2 significant digits.

Even products, which do not contain sensitizing substances or contain these substances in very low concentrations, may have a strong fragrance. It is not possible here to estimate the concentration or the content of the individual sensitizing substances in a product by smelling the product.

According to the declaration of contents product no. 7, which has the highest content of D-limonen, also has an orange fragrance or flavour. For the remaining products the content of fragrances do not correspond clearly with the flavour/fragrance listed on the product.

Methyl eugenol is not on the list of the 26 allergenic fragrances. However, the substance has been included in the analysis due to its carcinogenic effects effekt and because the amount of the subsatnce is regulated in the cosmetic directive (see 7.5 Health assessment of Methyl eugenol) and its natural occurrence in rose oil, which is found in three different products according to the INCI declarations.

6.5 Selection of substances for health assessment

The selection of fragrances for health assessment was based on occurrence in the products. Fragrances occurring in most products were selected for assessment. D-limonen and Benzyl alcohol have been assessed in a previous survey for the Danish Environmental Protection Agency, and besides these two substances the 4 fragrances found most often in the products were selected for health assessment. Methyl eugenol, analysed specifically for in 3 products, is also included in the assessment.

The five selected substances are: Linalool, Benzyl benzoate, Geraniol, Eugenol and Methyl eugenol.

| Front page | | Contents | | Previous | | Next | | Top |

Version 1.0 March 2006, © Danish Environmental Protection Agency