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

机译:基质固相分散-在线乙酰化气相色谱-质谱法测定海鲜中的对羟基苯甲酸酯类防腐剂

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摘要

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). (C) 2016 Elsevier B.V. All,rights reserved.
机译:提出了一种确定市售海鲜中四种常用的对羟基苯甲酸酯防腐剂(对羟基苯甲酸甲酯,对羟基苯甲酸乙酯,对羟基苯甲酸丙酯和对羟基苯甲酸丁酯)的有效方法。该方法在通过在线乙酰化气相色谱-质谱法(GC-MS)鉴定和定量对羟基苯甲酸酯防腐剂之前,采用基质固相分散体(MSPD)。通过Box-Behnken设计方法优化了影响MSPD提取效率的参数。在最佳条件下,将0.5 g的冷冻海鲜与0.5 g的无水硫酸钠混合,并通过涡旋与1.0 g的Florisil分散。之后,将共混物转移至含有1.5g硅胶+ C18(w / w,9:1)的玻璃柱中,该玻璃柱用作清洁助吸附剂。然后,目标分析物用12 mL乙腈洗脱。然后通过与乙酸酐的反应在GC进样口中在线衍生提取物,并通过GC-MS系统确定目标分析物的身份和数量。定量限(LOQ)为0.2至1.0 ng / g(干重)。初步结果显示,四种选定的对羟基苯甲酸酯的总浓度为16.7至44.7 ng / g(干重)。 (C)2016 Elsevier B.V.保留所有权利。

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