Determination of paraben preservatives in seafood using matrix solid-phase dispersion and on-line acetylation gas chromatography−mass spectrometry

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• 作者：Rosalina Djatmika^a ; ^b ; Chih-Chung Hsieh^a ; Jhih-Ming Chen^a ; Wang-Hsien Ding^a ; ^{wanghsiending@gmail.com" class="auth_mail" title="E-mail the corresponding author}
• 关键词：Paraben preservatives ; On-line acetylation ; Matrix solid-phase dispersion ; GC&ndash ; MS ; Biota sample analysis
• 刊名：Journal of Chromatography B, Analytical Technologies in the Biomedical and Life Sciences
• 出版年：2016
• 出版时间：15 November 2016
• 年：2016
• 卷：1036-1037
• 期：Complete
• 页码：93-99
• 全文大小：999 K

文摘

An effective method for determining four commonly detected paraben preservatives (methyl, ethyl, propyl and butyl paraben) in marketed seafood is presented. This method employs matrix solid-phase dispersion (MSPD) before identification and quantification of the paraben preservatives via on-line acetylation gas chromatography–mass spectrometry (GC–MS). Parameters affecting the extraction efficiency of MSPD were optimized through a Box-Behnken design method. Under optimal condition, 0.5-g of freeze-dried seafood was mixed with 0.5-g of anhydrous sodium sulfate, and dispersed with 1.0-g of Florisil using vortex. After that, the blend was transferred to a glass column containing 1.5-g of silica gel + C18 (w/w, 9:1), which acted as clean-up co-sorbents. Then, target analytes were eluted with 12 mL of acetonitrile. The extract was then derivatized on-line in the GC injection-port through reaction with acetic anhydride, and the identity and quantity of the target analytes were determined by the GC–MS system. The limits of quantitation (LOQs) were 0.2 to 1.0 ng/g (dry weight). Preliminary results showed that the total concentrations of four selected parabens ranged from 16.7 to 44.7 ng/g (dry weight).