|
| Front page | | Contents | | Previous | | Next |
Survey and health risk assessment of products for treatment of sports injuries and pains
3 Quantitative chemical analyses
3.1 Quantitative determination of volatile and semi volatile compounds (GC/MS screening)
In consultation with the Danish EPA a number of substances were selected for quantification. As the method used in connection with the screening was not a suitable analysis method for quantification of contents of organic substances, it was decided to use Solid Phase Micro Extraction (SPME) as sampling principle combined with GC/MS.
3.1.1 Method for quantitative SPME-GC/MS analysis
The sample was weighed out in a 20 ml membrane glass. 3 different isotope- marked, internal standards (Toluene-d8, phenol-d6 and naphthalene-d8) were added to the sample. Headspace was sampled for 15 min. at SPME and subsequently analysed by gas chromatography/mass spectrometry (GC/MS). The parameters were as follows:
Table 3.1 Parameters for SPME-GC/MS analysis
| GC/MS-Instrument |
Thermo Finnigan, DSQ |
| MS-parameters |
Autotune, 35-300 m/z, solvent delay: 4,0 min. |
| GC-parameters |
Furnace prog: 40 ° C for 1 min., 10 ° C/min. To 260 ° C hold for 2 min.
Injector: 290 ° C, splitless time: 0.5 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 |
Calibration of the method has been carried out at 6 different concentration levels from 0.1 to 50 μg per headspace glass.
The detection limit of the method was determined to 1 mg/kg and the uncertainty is between 10-25 % RSD, depending on the substance.
3.1.2 Results of SPME-GC/MS-analysis in mg/kg
The quantified contents of the GC/MS analysis are listed in below tables.
Table 3.2 SPME-GC/MS analysis results in mg/kg
| Substance |
CAS no. |
Sample marking |
| 1 |
2 |
3 |
4 |
5 |
8 |
| Toluene |
89-83-8 |
<1 |
3.0 |
<1 |
<1 |
<1 |
2.3 |
| Dimethyl sulphone |
67-71-0 |
<1 |
<1 |
<1 |
<1 |
<1 |
<1 |
| Benzaldehyde |
100-52-7 |
<1 |
4,200 |
<1 |
<1 |
<1 |
<1 |
| α-Pinene |
7785-70-8 |
<1 |
12.000 |
550 |
1.700 |
<1 |
27.000 |
| Phenol |
108-95-2 |
<1 |
<1 |
<1 |
2.4 |
5.6 |
11 |
| Camphene |
79-92-5 |
<1 |
360 |
3.4 |
300 |
<1 |
130 |
| Benzyl alcohol |
100-51-6 |
<1 |
9.2 |
<1 |
<1 |
<1 |
<1 |
| p-Methylanisol |
104-93-8 |
<1 |
<1 |
<1 |
<1 |
<1 |
<1 |
| 3-Carene |
13466-78-9 |
<1 |
240 |
1.7 |
290 |
<1 |
<1 |
| d-Limonene |
5989-27-5 |
9.8 |
19.000 |
400 |
1.500 |
<1 |
1.000 |
| Linalool |
78-70-6 |
2,2 |
1.900 |
93 |
1.000 |
<1 |
100 |
| Camphor |
21368-68-3 |
5,3 |
77.000 |
5.100 |
980 |
<1 |
8,2 |
| Methyl salicylate |
119-36-8 |
51.000 |
5300 |
6,4 |
<1 |
<1 |
50.000 |
| Estragole |
140-67-0 |
<1 |
<1 |
<1 |
<1 |
<1 |
11 |
| 2-Phenoxy ethanol |
122-99-6 |
390 |
<1 |
9.000 |
<1 |
4.900 |
680 |
| Cinnamale |
104-55-2 |
<1 |
10.000 |
<1 |
<1 |
<1 |
<1 |
| Eugenol |
97-53-0 |
<1 |
27.000 |
<1 |
<1 |
<1 |
<1 |
| Isoeugenol |
97-54-1 |
<1 |
1.600 |
<1 |
<1 |
<1 |
<1 |
| Substance |
CAS no. |
Sample marking |
| 12 |
13 |
15 |
C |
E |
H |
| Toluene |
89-83-8 |
<1 |
<1 |
1,7 |
<1 |
2,6 |
4,4 |
| Dimethyl sulphone |
67-71-0 |
<1 |
8.200 |
8.0 |
57 |
<1 |
<1 |
| Benzaldehyde |
100-52-7 |
<1 |
<1 |
<1 |
2.0 |
<1 |
<1 |
| α-Pinene |
7785-70-8 |
<1 |
16 |
19.000 |
<1 |
33.000 |
22.000 |
| Phenol |
108-95-2 |
<1 |
16 |
4.4 |
<1 |
6.5 |
2.0 |
| Camphene |
79-92-5 |
<1 |
<1 |
48 |
<1 |
47 |
150 |
| Benzyl alcohol |
100-51-6 |
<1 |
7.3 |
<1 |
<1 |
<1 |
<1 |
| p-Methylanisol |
104-93-8 |
<1 |
9.5 |
<1 |
<1 |
<1 |
<1 |
| 3-Carene |
13466-78-9 |
<1 |
<1 |
<1 |
<1 |
<1 |
<1 |
| d-Limonene |
5989-27-5 |
1.1 |
1.1 |
170 |
44 |
2.300 |
870 |
| Linalool |
78-70-6 |
<1 |
43 |
30 |
6.3 |
1.700 |
1.800 |
| Camphor |
21368-68-3 |
2.500 |
<1 |
9.0 |
<1 |
<1 |
<1 |
| Methyl salicylate |
119-36-8 |
<1 |
<1 |
45.000 |
<1 |
67.000 |
76.000 |
| Estragole |
140-67-0 |
<1 |
<1 |
8.0 |
<1 |
10 |
14 |
| 2-Phenoxy ethanol |
122-99-6 |
<1 |
410 |
<1 |
<1 |
<1 |
<1 |
| Cinnamale |
104-55-2 |
<1 |
<1 |
<1 |
<1 |
<1 |
<1 |
| Eugenol |
97-53-0 |
<1 |
<1 |
<1 |
<1 |
<1 |
<1 |
| Isoeugenol |
97-54-1 |
<1 |
<1 |
<1 |
<1 |
<1 |
<1 |
”<1” means that the content is lower than the detection limit for the applied analysis method. (1mg/kg)
3.2 Specific analysis of contents of organic solvents
With the applied SPME-GC/MS analysis it was not possible to carry out a quantification of the contents of the identified organic solvents and a GC/FID-based method was therefore developed for the purpose.
3.2.1 Method for quantitative analysis of organic solvents
Following parameters were applied for the specific analysis of organic solvents.
Table 3.3 Analysis parameters for GC/FID based method
| GC-Instrument |
HP 5890 |
| GC-parameters |
Furnace progr: isotherm at 80° C.
Injector: 225° C, FID-detector: 225° C
Carrier gas: Nitrogen, constant flow: 25 ml/min.
Column: 4 m, 10 % carbowax 1500 |
| Solvent |
Dimethylformamide (DMF) |
3.2.2 Results of the specific analysis of organic solvents
Table 3.4 lists the identified contents
Table 3.4 Results of specific analysis of organic solvents
| Substance |
CAS no. |
Sample marking |
| 1 |
2 |
3 |
4 |
5 |
8 |
12 |
13 |
15 |
C |
E |
H |
| Toluene* |
89-83-8 |
|
3 ppm |
|
|
|
2.3 ppm |
|
|
1.7 ppm |
2.6 ppm |
|
4.4 ppm |
| Ethanol |
64-17-5 |
|
|
|
54% |
2.2% |
|
|
|
|
14% |
|
|
| 2-Propanol |
67-63-0 |
|
|
|
|
|
|
27% |
|
|
|
|
|
| Tert-butanol |
75-65-0 |
|
|
|
|
|
|
|
|
|
0.35% |
|
|
| Acetone |
67-64-1 |
|
|
|
|
|
|
|
|
|
1.9% |
|
|
Empty fields = The solvent was not found in the sample
* The content of toluene is determined by SPME-GC/MS see paragraph SPME-GC/MS 3.1.1.
3.3 Prioritisation of substances in products for treatment of sport injuries and pain
Based on the screening of health effects and the qualitative analysis a number of results has been selected for health assessment.
The most interesting substance has been selected in co-operation with the danish environmental protection agency.
- Camphor
- Dimethyl sulphone
- D-limonen
- Methyl salicylat
- 2-phenoxyethanole
- α-Pinene
Furthermore the following solvents has been selected
- Etanol
- 2-Propanol
- Acetone
- T-Butyl alcohol
| Front page | | Contents | | Previous | | Next | | Top |
Version 1.0 Decmeber 2006, © Danish Environmental Protection Agency
|