| Titre : |
Accurate and simple method for simultaneous determination of restricted ethylene glycol ethers and esters in leather by GC-MS |
| Type de document : |
texte imprimé |
| Auteurs : |
He-Wei Ma, Auteur ; Luo Jian-Xun, Auteur |
| Année de publication : |
2021 |
| Article en page(s) : |
p. 117-123 |
| Note générale : |
Bibliogr. |
| Langues : |
Anglais (eng) |
| Catégories : |
Chimie analytique
Chromatographie en phase gazeuse
Cuirs et peaux -- Analyse
Esters
Ethers
Ethylène glycol
Extraction (chimie)
Spectrométrie de masse
|
| Index. décimale : |
675 Technologie du cuir et de la fourrure |
| Résumé : |
An analytical approach was developed for the simultaneous determination of the eight ethylene glycol ethers (EGEs) and esters (EGEEs) prohibited by European Union (EU) REACH regulation in leather samples. The analytes were extracted using methanol with ultrasonic assistance within 30 minutes. The extracts were cleaned up by passing the extraction solution through a cartridge containing alumina-N frits, and the eluate was injected into GC-MS which was fitted with a 60m length capillary DB-WAX column. Excellent separation of the eight EGEs/EGEEs was achieved by the capillary column within 25 minutes. The clean-up with Alumina-N cartridge presented desired efficiency for removing the co-extractives in the extracts. The major advantages of this method are the simplicity and accuracy. Limitation of the detection, linear range, and reproducibility of the method were evaluated. Average recoveries in the range of 91.7%-102.5% (RSD, <6.1 0/0) with detection limits at 3.09.4mg/kg for the eight targets were obtained. Analytical results showed that ethylene glycol dimethyl ether (EGDME), ethylene glycol ethyl ether (EGEE), and diethylene glycol dimethyl ether (DEGDME), were found in 22% of 95 leather samples at the concentration range of 35-82mg/kg, 12-285mg/kg and 28-66mg/kg, respectively, while the other five EGEs/EGEEs were not detected. |
| Note de contenu : |
- EXPERIMENTAL PROCEDURES : Chemicals - Apparatus - Preparation and storage of standards - Sampling - Sample extraction - Extract clean-up - Instrumental analysis
- RESULTS AND DISCUSSION : Selection of capillary column - Sample preparation - Effects of extraction time and temperature
- METHOD VALIDATION : Linearity - Limits of detection (LOD) and quantification (LOQ) - Reproducibility studies - Analysis of leather samples
- Table 1 : EGEs and EGEEs used in the experiment : Name, abbreviation, CAS N°., boiling point and monitored ions (m/z)
- Table 2 : Recoveries of eight EGEs/EGEEs by the three SPE cartridges
- Table 3 : Recoveries in the spiked negative leather with different temperature and time
- Table 4 : Effects of MgSO4 used in the extraction process on the test results
- Table 5 : Calibration data, precision and detection limits for the selected compounds
- Table 6 : Levels of the prohibited EGEs/EGEEs found in leather samples |
| En ligne : |
https://drive.google.com/file/d/1N6bhRrkh3wBBN1EUu33c6Tv8ADpSMiXw/view?usp=drive [...] |
| Format de la ressource électronique : |
Pdf |
| Permalink : |
https://e-campus.itech.fr/pmb/opac_css/index.php?lvl=notice_display&id=35831 |
in JOURNAL OF THE SOCIETY OF LEATHER TECHNOLOGISTS & CHEMISTS (JSLTC) > Vol. 105, N° 3 (05-06/2021) . - p. 117-123
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