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

Survey and health assesment of chemicals substances in pleasure gel

3 Quantitative chemical analyses

3.1 Quantitative determination of volatile and semi-volatile compounds

The same analysis principle was used as in connection with qualitative screening, SPME combined with GC/MS. However, in connection with quantitative measurements another SPME fibre with greater capacity was used. The application of this SPME fibre was necessary in order to carry out the quantification which simultaneously resulted in reduced sensitivity of the analysis method compared to the applied method during screening. Due to these conditions, individual components identified in connection with the qualitative examination could not be quantified.

Three different isotope marked internal standards were added to the sample (toluen-d8, phenol-d6 and naphthalen-d8).

The method was calibrated at 6 different levels of concentration from 0.1 to 50 µg per headspace glass.

The sample was weighed in a 20 ml membrane glass. Different amounts were weighed depending on the content of organic components in the investigated products from 0.05 g to 0.05 mg sample per headspace glass. Headspace was sampled for 15 min. at SPME and subsequently analysed at gas chromatography with mass spectrometric detection (GC/MS). The following parameters were applied:

GC/MS Instrument Thermo Finnigan, DSQ
MS parameters Autotune, 35-300 m/z, solvent delay: 4.0 min.
GC parameters Oven prog: 40 °C for 1 min., 10 °C/min. to 260 °C hold for 2 min.
Injector: 290 °C, splitless time: 0.50 min.
Carrier gas: Helium, constant flow: 1.0 ml/min.
Column: Valcobond VB-1, 30 m x 0.25 mm, film: 1.5 µm
SPME parameters Fibre: 100 µm PDMS
Headspace temperature: 35 °C

The detection limit: 1 mg/kg. Analysis uncertainty: 10-25 % RSD, depending on component.

3.2 Analysis results

The quantified contents from the performed GC/MS analysis appear from Table 3.1.

Please note that product no. 24 merely was included in the quantitative measurement as it could not be procured earlier in the project. The product consists of 3 different flavours (in the same package) and only one variety was analysed.

Table 3.1 Results from GC/MS screening of pleasure gel

Component Sample marking [mg/kg]
1 2 3 4 6 7 8 9 11 12 13
1-Phenoxy propan-2-ol <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1
2-Phenoxyethanol 2,500 1,400 <1 <1 <1 <1 8,300 <1 6,800 7,000 5,100
3-Caren <1 <1 <1 <1 16 <1 <1 <1 <1 <1 <1
α-Pinene <1 <1 1,2 <1 260 <1 <1 <1 <1 <1 <1
Benzaldehyde <1 17 <1 28 200 4,0 <1 <1 <1 <1 <1
Benzyl acetate 6.5 2,400 3.1 <1 <1 3.5 <1 <1 2.8 3.8 2.7
Benzyl alcohol <1 9.6 <1 45 140 <1 <1 <1 <1 <1 <1
Camphen <1 <1 <1 <1 46 <1 <1 <1 <1 <1 <1
Camphor <1 <1 <1 <1 900 <1 <1 <1 <1 <1 <1
Cinnamal <1 <1 <1 6,200 17,000 270 <1 <1 <1 <1 <1
Cinnamyl alcohol <1 <1 <1 12 <1 <1 <1 <1 <1 <1 <1
Citral <1 <1 <1 <1 <1 40 <1 <1 <1 <1 <1
Citronellal <1 <1 <1 <1 <1 240 <1 <1 <1 <1 <1
Citronellol <1 <1 <1 <1 <1 180 <1 <1 <1 <1 <1
Coumarin <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1
Dehydro acetic acid 9.2 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1
D-Limonene <1 <1 4.9 56 400 20 <1 <1 <1 <1 <1
Estragole <1 <1 3.0 5,500 <1 <1 <1 <1 <1 <1 <1
Eugenol <1 <1 <1 500 18,000 380 <1 <1 <1 <1 <1
Hexyl cinnemaldehyde <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1
Hydroxy citronellal <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1
Isoeugenol <1 <1 <1 8,3 500 18 <1 <1 <1 <1 <1
Linalool <1 1,400 <1 200 1,200 9.0 <1 <1 <1 <1 <1
Methyl salicylate <1 1.5 <1 <1 <1 <1 <1 <1 <1 <1 <1
Phenol 8.4 1.8 1.5 <1 <1 <1 10 2.3 5.3 7.5 4.6
p-Methylanisol <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1
P-Propenyl anisol <1 <1 64 <1 43 <1 <1 <1 <1 <1 <1
Pyrazin <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1
Toluen <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1

”<1” means that the content is less than the detection limit of the applied analysis method.

Table 3.1 - continued – Results from GC/MS screening of pleasure gel

Component Sample marking [mg/kg]
15 18 21 22 23 24 25 27 29 30 32
1-Phenoxy propan-2-ol <1 <1 <1 23 <1 <1 <1 <1 <1 <1 <1
2-Phenoxyethanol <1 61 <1 <1 1,300 100,000 <1 <1 <1 <1 <1
3-Caren <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1
a-Pinen <1 <1 <1 <1 <1 <1 <1 <1 <1 560 <1
Benzaldehyde <1 <1 <1 <1 <1 6.3 <1 16 6.1 71 5.0
Benzyl acetate 40 <1 5.2 4.6 3.9 96 5.5 290 300 480 250
Benzyl alkohol <1 <1 <1 <1 <1 1.9 <1 22 6.2 <1 17
Camphen <1 <1 <1 <1 <1 <1 <1 <1 15 <1 <1
Camphor <1 <1 <1 <1 <1 <1 3.9 <1 <1 <1 <1
Cinnamal <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1
Cinnamyl alkohol <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1
Citral <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1
Citronellal <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1
Citronellol <1 <1 <1 <1 <1 <1 <1 340 <1 <1 210
Coumarin 36 <1 <1 <1 <1 <1 <1 190 <1 <1 460
Dehydro acetic acid <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1
D-Limonene 8.1 <1 <1 <1 <1 <1 <1 150 51 220 23
Estragole <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1
Eugenol <1 <1 <1 <1 <1 <1 <1 830 <1 <1 <1
Hexyl Cinnamaldehyde <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1
Hydroxy citronellal <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1
Isoeugenol <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1
Linalool 36 <1 <1 <1 <1 <1 <1 1,300 99 1,400 340
Methyl salicylate <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1
Phenol 4.6 1.0 2.2 20 7.1 19 3.3 2.7 2.5 1.7 1.7
p-Methylanisol <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 18
P-Propenyl anisol <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1
Pyrazin <1 <1 <1 <1 <1 <1 2.4 <1 <1 <1 <1
Toluen <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1

”<1” means that the content is less than the detection limit of the applied analysis method.

Detection limit: 1 mg/kg. Analysis uncertainty: 10-25 % RSD, depending on the component.

3.3 Order of priority of substances in pleasure gel

In the light of the performed health screening and the quantitative analysis, a number of substances were chosen for additional health assessment.

It was estimated that the most interesting substances are:

  • Eugenol
  • Cinnamal
  • Linalool
  • 2-phenoxyethanol
  • D-Limonene.

Furthermore, there are substances that were estimated in connection with the survey of sports creams and the following substances are relevant for pleasure gels:

  • Camphor
  • α-Pinene.

 

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



Version 1.0 September 2006, © Danish Environmental Protection Agency