Simultaneous gas chromatography-mass spectrometric determination of total and individual phthalic esters utilizing alkaline hydrolysis and silyl derivatization technique SCIE SCOPUS KCI

Cited 6 time in WEB OF SCIENCE Cited 7 time in Scopus
Title
Simultaneous gas chromatography-mass spectrometric determination of total and individual phthalic esters utilizing alkaline hydrolysis and silyl derivatization technique
Author(s)
Kim, Minseon; Li, Donghao; Shim, Won-Joon; Oh, Jae-Ryoung; Park, Jongman
KIOST Author(s)
Shim, Won Joon(심원준)Oh, Jae Ryoung(오재룡)
Publication Year
2007-03-20
Abstract
Environmentally important phthalic esters have been analyzed by GC-MS in terms of individual phthalic esters or total phthalic esters directly or after derivatization. Derivatization improves the chromatographic characteristics of the highly polar phthalic esters. This study focused on the GC-MS determination of the total phthalic esters and the individual plithalic esters simultaneously. The plithalic esters were hydrolyzed to phthalate and corresponding alcohols in 1 M NaOH solution at 90 degrees C for 30 min followed by extraction with ethyl acetate after acidifeation. The phthalic acid and alcohols were simultaneously silyl derivatized using bis(trimethylsilyl)trifluoroacetamide (BSTFA) to their corresponding silyl ester and ethers in the mixture of 60% acetone and 40% ethyl acetate at room temperature within 30 min. Because of the high reactivity of BSTFA with the plithalic acid and alcohols effective silyl derivatization was possible simultaneously. GC-MS analysis of the silyl derivatives of phthalic acid and alcohols was performed. The total plithalic ester content was estimated from the analytical result of phthalic silyl ester, while the individual plithalic ester was quantified from the analytical results of alcoholic silyl ethers. This technique was applied to spiked tab water and real seawater samples from the Lake Shihwa in Korea. The results were checked against the results from the direct GC-MS analysis of the phthalic esters and reasonable recoveries with high sensitivity were achieved. The recoveries were higher than 75% with low relative standard deviation (below 10%).
ISSN
0253-2964
URI
https://sciwatch.kiost.ac.kr/handle/2020.kiost/4717
Bibliographic Citation
BULLETIN OF THE KOREAN CHEMICAL SOCIETY, v.28, no.3, pp.432 - 438, 2007
Publisher
KOREAN CHEMICAL SOC
Subject
SOLID-PHASE MICROEXTRACTION; LIQUID-CHROMATOGRAPHY; DI(2-ETHYLHEXYL) PHTHALATE; ELECTRON-CAPTURE; WATER SAMPLES; BISPHENOL-A; GC-MS; ACID; EXTRACTION; PLASMA
Keywords
total phthalic esters; silyl derivatization; plasticizer
Type
Article
Language
English
Document Type
Article
Publisher
KOREAN CHEMICAL SOC
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