US EPA

8312166 

Meetings & Symposia 

Determination of nonylphenol ethoxylates in leather by GC-MS pretreated with cleavage of hydroiodic acid and the feasibility 

Ma, H; Huang, X; Zhu, G; Zhang, D 

2013 

Deri Teknologlari, Teknisyenleri ve Kimyacilari Dernegi 

32nd Congress of the International Union of Leather Technologists and Chemist Societies, IULTCS 2013 

English 

Nonylphenol ethoxylates (NPEOn) residue is considered to be a ubiquitous pollutant in leather. The related test techniques have attracted wide attention. However, no popular methods have been developed for NPEOn test in leather. Therein, the test method of NPEOn is one of the main research directions in analytical field. In this paper, an analytical method for the determination of NPEOn in leather was studied. The method combined an ultrasonic assisted extraction procedure, an enrichment step onto C18 solid phase extraction (SPE) treatment and cleavage process with hydroiodic acid prior to analysis using gas chromatography mass spectrometry (GC-MS). Method validation of each process was carried out by recovery evaluation. 5 g leather samples were extracted assisted by sonication in two consecutive steps of 30 min using 100 ml methanol. 10 ml of the obtained extracts were mixed with 10 ml water and loaded onto C18 cartridges and analytes were eluted with 3 × 2 ml methanol. The elution was evaporated and treated by 20 ml hydroiodic acid (37%) with 4 g sodium hypophosphite at 100°C for 24 h. Finally, NP in the cleavage resultants was extracted with hexane and analyzed by GC-MS. The results presented that the procedures performed low quantitative recoveries mainly due to the fact that NPEOn was not transformed to NP with equal moles during the cleavage process. Further improvement and optimization of the cleavage conditions should be done for the application of the proposed method to quantitatively determine NPEOn residues in leather by GC-MS. 

Cleavage; GC-MS; Hydroiodic acid; Leather; Nonylphenol ethoxylates