College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou, Zhejiang, PR China.
J Sep Sci. 2013 Jul;36(14):2268-76. doi: 10.1002/jssc.201300239. Epub 2013 Jun 21.
Derivatization at the injection port following hollow-fiber-based liquid-liquid-liquid microextraction with tetramethylammonium acetate as a dual-function reagent, i.e. an acceptor and derivatization reagent, for the determination of benzoic acid (BA) and sorbic acid (SA) in real samples by GC was developed. BA and SA were extracted from aqueous samples to an organic phase impregnated into the pores of the hollow fiber wall, and then back-extracted to the acceptor solution located inside the lumen of the hollow fiber. Upon injection, the extracted analytes were quantitatively derivatized to their methyl esters with tetramethylammonium acetate in the GC injection port. Several parameters related to the derivatization and extraction efficiency were optimized. The linearity was satisfactory over a concentration range of 0.1-50 mg/L with r > 0.993 for both analytes. The LODs were 2.0 μg/L for SA and 20 μg/L for BA. The recoveries (83-116%) and precisions (RSDs of 1.2-11.4% (n = 3)) were examined by analyzing real spiked samples. The enrichment factors of BA and SA were 300 and 425. The results demonstrated that this is a simple, rapid, accurate, and sensitive method for the determination of BA and SA in various samples.
以四甲基乙酸铵为双重功能试剂(即接受体和衍生化试剂),通过 GC 在注射口进行衍生化,开发了基于中空纤维的液 - 液 - 液微萃取法,用于测定实际样品中的苯甲酸(BA)和山梨酸(SA)。BA 和 SA 从水样中被萃取到有机相中,然后再反萃取到位于中空纤维内腔中的接受体溶液中。进样时,在 GC 进样口中,萃取的分析物与四甲基乙酸铵定量衍生化为甲酯。优化了与衍生化和萃取效率相关的几个参数。两种分析物的浓度范围在 0.1-50 mg/L 之间,线性良好,r > 0.993。SA 的检出限为 2.0 μg/L,BA 的检出限为 20 μg/L。通过分析实际加标样品来检验回收率(83-116%)和精密度(RSD 为 1.2-11.4%(n = 3))。BA 和 SA 的富集因子分别为 300 和 425。结果表明,这是一种简单、快速、准确、灵敏的方法,可用于测定各种样品中的 BA 和 SA。