Silyl derivatization of alkylphenols, chlorophenols, and bisphenol A for simultaneous GC/MS determination
Silyl derivatization of alkylphenols, chlorophenols, and bisphenol A for simultaneous GC/MS determination
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DOI：
10.1021/ac001494l
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发表时间：
2001-07-01
影响因子：
7.4
通讯作者：
Oh, JR
中科院分区：
文献类型：
--
作者：
Li, D;Park, J;Oh, JR
建立了一种同时分析烷基酚、氯酚和双酚A的快速硅基衍生化技术。用过量的双（三甲基硅基）三氟乙酰胺（BSTFA）将分析物硅化，然后用水水解多余的硅基试剂。在各种溶剂中研究了衍生化反应的速率，发现在丙酮中反应速度最快。在丙酮中衍生化反应在室温下15 s内定量完成，而在其他溶剂中则需要1 h以上。当丙酮含量大于60% （v/v）时，在丙酮混合溶剂中也可得到类似的结果。由于水不混溶溶剂如二氯甲烷或己烷经常用于各种样品基质中酚类分析物的提取，因此可以在提取物中加入丙酮以加快衍生化反应的速度，通过将多余的衍生化试剂BSTFA水解，然后用无水硫酸钠脱水，以确保样品中衍生物的稳定性，以长期储存。在此基础上，设计衍生化处理试剂盒，提高分析的便捷性。使用该试剂盒可以在几分钟内成功处理样品。因此，采用气相色谱/质谱法快速同时测定这些分析物具有较高的方便性、灵敏度和重现性。
A fast silyl derivatization technique for simultaneous GC/MS analysis of alkylphenols, chlorophenols, and bisphenol A was developed. The analytes were silylized with an excess amount of bis(trimethylsilyl)trifluoroacetamide (BSTFA) followed by hydrolysis of excess silyl reagent with water. Reaction rates of derivatization were studied in various solvents and found to be fastest in acetone. Derivatization reaction in acetone was completed quantitatively within 15 s at room temperature while it took more than 1 h in other solvents studied. Similar results were obtained in mixed solvents with acetone if the content of acetone was higher than 60% (v/v). Since water-immiscible solvents such as dichloromethane or hexane are frequently used in the extraction of phenolic analytes in various sample matrixes, acetone can be added to the extracts in order to accelerate the reaction rate of derivatization, Stability of the derivatives in sample for long-term storage was ensured by hydrolyzing excess derivatizing reagent, BSTFA, with a spike of water followed by dehydration using anhydrous sodium sulfate. On the basis of the above results, a derivatizing treatment kit was designed to improve the convenience of analysis. It was possible to treat sample within several minutes successfully by using the kit. So fast simultaneous determination of those anlaytes by GC/MS was possible with improved convenience as well as sensitivity and reproducibility.