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Simultaneous Gas Chromatography-Mass Spectrometric Determination of Total and Individual Phthalic Esters Utilizing Alkaline Hydrolysis and Silyl Derivatization Technique
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  • Simultaneous Gas Chromatography-Mass Spectrometric Determination of Total and Individual Phthalic Esters Utilizing Alkaline Hydrolysis and Silyl Derivatization Technique
  • Simultaneous Gas Chromatography-Mass Spectrometric Determination of Total and Individual Phthalic Esters Utilizing Alkaline Hydrolysis and Silyl Derivatization Technique
저자명
Kim. Min-Seon,Li. Dong-Hao,Shim. Won-Joon,Oh. Jae-Ryoung,Park. Jong-Man
간행물명
Bulletin of the Korean Chemical Society
권/호정보
2007년|28권 3호|pp.432-438 (7 pages)
발행정보
대한화학회
파일정보
정기간행물|ENG|
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이 논문은 한국과학기술정보연구원과 논문 연계를 통해 무료로 제공되는 원문입니다.
서지반출

기타언어초록

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 phthalic esters simultaneously. The phthalic esters were hydrolyzed to phthalate and corresponding alcohols in 1 M NaOH solution at 90 oC for 30 min followed by extraction with ethyl acetate after acidifcation. 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 phthalic 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 phthalic ester content was estimated from the analytical result of phthalic silyl ester, while the individual phthalic 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%).