Quantitative Silylation Speciations of Primary Phenylalkyl Amines, Including Amphetamine and 3,4-Methylenedioxyamphetamine Prior to Their Analysis by GC/MS
作者:Borbála Molnár、Blanka Fodor、Imre Boldizsár、Ibolya Molnár-Perl
DOI:10.1021/acs.analchem.5b02599
日期:2015.10.20
nitrogen prior to their injection. Efficiences of the novel catalyzed trimethylsilylation (MSTFA) and our recently introduced (now, for A and MDA extended) acylation principle were contrasted. Catalyzed trimethylsilylation led to diTMS derivatives resulting in on average a 1.7 times larger response compared to the corresponding acylated species. Catalyzed trimethylsilylation of PPAAs, A, and MDA were characterized
注意到一种新颖的定量三甲基甲硅烷基化方法,可衍生11种伯苯烷基胺(PPAA),包括苯丙胺(A)和3,4-亚甲二氧基苯丙胺(MDA)。用N-甲基-N触发完全衍生化的二三甲基甲硅烷基(diTMS)物种-(三甲基甲硅烷基)-三氟乙酰胺(MSTFA)试剂,随后通过GC / MS识别了新原理。在方法优化过程中,研究了溶剂(乙腈,ACN;乙酸乙酯,ETAC;吡啶,PYR)和催化剂(三甲基氯硅烷,TMCS;三甲基碘硅烷,TMIS)的互补影响:溶剂和催化剂的作用被证明是同等的至关重要的。使用MSTFA / PYR = 2 / 1–9 / 1(v / v)的试剂施加催化剂可获得最佳的,成比例的,巨大的响应。A和MDA需要TMIS,而其余的PPAA向diTMS产品也提供TMCS。类似于Molnar等用六甲基二和全氟羧酸(HMDS和PFCA)生成的衍生物(Anal.Chem.31:426-428中。 2015年