Automated derivatization for on-line solid-phase extraction-gas chromatography; phenolic compounds

✍ Scribed by Louter, Arjan J. H. ;Jones, Philo A. ;Jorritsma, J. David ;Vreuls, Jolan J. ;Brinkman, Udo A. Th.

• Publisher: John Wiley and Sons
• Year: 1997
• Tongue: English
• Weight: 619 KB
• Volume: 20
• Category: Article
• ISSN: 0935-6304
• DOI: 10.1002/jhrc.1240200704

✦ Synopsis

Abstract

An automated system for derivaatization was coupled on‐line with solid‐phase extraction‐gas‐chromatography (SPE‐GC). The system was optimized for the determination of phenol and chlorinated phenols in aqueous samples. The test analytes were acetylated with acetic anhydride; proper buffering of the sample was a critical factor. Next, the phenol acetates were enriched on a SPE cartridge and transferred to a GC; two appraoaches were studied. In the first approach, the derivatives were enriched on disposable C18 cartridges (ASPEC type) and desorbed with methylacetate. Aan aliquot of the final eluate was injected on‐line the GC by means of a loop‐type interface. In the second approach, trace enrichment was performed on 10 × 2 mm i.d. LC‐type precolumn packed with polystyrenedivinylbenzene copolymer (PLRP‐S) this precolumn was dried with a mitrogen purge and the phenol acetates were desorbed with ethyl acetate which was injectedon‐line into the retention gap of the GC under partially concurrent solvent evaporation (PCSE) conditions. The Derivatization‐SPE‐GC system which was based on the loop‐type interface has the advantage of simplicity and easy operation, the main drawback is the impossibility to determine phenol acetates which elute prior to trichlorophenol acetates. With the derivatization‐SPE‐GC approach using PCSE‐based desorption, even the most volatile analyte of the test series, phenol acetate, can be determined successfully. The entire procedure, including the derivatization step, was fully automated and integrated in one set‐up. The precision data for the integrated on‐line derivatization‐SP‐FID system were fully satisfactory, with RSD values of 1–12 % at the 1 μg/1 level. When a sample volume of 2.2 ml was analyzed, The detection limits for the chlorinated phenol acetates were in the 0.1–0.3 μg/1 range.