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基于BSTFA衍生/GC-MS与DLLME/HPLC的老化变压器油中短碳链羧酸的分析
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李海燕,华佳,王逸凡,杨珍,李吟霜 中南民族大学化学与材料科学学院分析化学国家民委重点实验室 
基金项目:中国电力科学研究院科研项目(151000637)
中文摘要:以N,O-双(三甲基硅烷基)三氟乙酰胺(BSTFA)为硅烷化试剂,建立了衍生化气相色谱-质谱(GC-MS)测定老化变压器油中短链羧酸的定性分析方法;并建立了分散液液微萃取/高效液相色谱(DLLME/HPLC)测定其中甲酸、乙酸和糠酸的定量分析方法。结果表明:以乙腈为萃取剂,BSTFA为硅烷化试剂,60 ℃下反应60 min后进行GC-MS测定,在老化变压器油中检出甲酸、乙酸和糠酸等14种短碳链羧酸。以水为萃取剂对标准油样中的甲酸、乙酸和糠酸进行萃取,取水萃取相直接进行HPLC测定。在最佳条件下,甲酸、乙酸在0.05~50.0 mg/L及糠酸在0.01~2.0 mg/L质量浓度范围内线性良好,相关系数(r)大于0.998,检出限(LOD)分别为36.1、47.3、7.0 μg/L,相对标准偏差(RSD)分别为2.4%、3.3%和3.6%,3种羧酸的富集倍数为8~10倍。老化油样的加标回收率为91.7%~107%。该法简单有效,为变压器油纸绝缘老化特征量的正确使用和羧酸类物质对油纸绝缘老化影响的研究提供了数据。
中文关键词:硅烷化衍生  气相色谱-质谱(GC-MS)  短碳链羧酸  分散液液微萃取  高效液相色谱  变压器油
 
Analysis of Short-chain Carboxylic Acids in Aged Transformer Oil Based on BSTFA Derivatization/GC-MS and DLLME/HPLC
Abstract:An analytical method was established for the confirmation and quantitation of short chain carboxylic acids in aged transformer oil by gas chromatography-tandem mass spectrometry(GC-MS)and high performance liquid chromatography with dispersive liquid-liquid microextraction(DLLME/HPLC).The short-chain carboxylic acids in aged transformer oil were detected by GC-MS using N,O-bis-(trimethylsilyl)-trifluoroacetamide(BSTFA)as silane derivatization reagent,and formic acid,acetic acid and furoic acid in transformer oil were quantified by DLLME/HPLC.After extracting carboxylic acid in transformer oil with acetonitrile as extractant,BSTFA was added into the extraction phase of acetonitrile for silylation derivatization.After 60 min of the reaction at 60 ℃,the samples were determined by GC-MS.Results showed that 14 kinds of short chain carboxylic acids were detected in heat aged transformer oil,including formic acid,acetic acid and furoic acid.The formic acid,acetic acid and furoic acid in the standard oil sample were extracted with water as extractant which was directly taken for injection.The calibration curves of formic acid,acetic acid and furoic acid in the transformer oil were linear in the ranges of 0.05-50.0 mg/L,0.05-50.0 mg/L and 0.01-2.0 mg/L,respectively,with correlation coefficients(r) more than 0.998.The limits of detection(LOD) of the method were 36.1,47.3 and 7.0 μg/L,with relative standard deviations(RSD) of 2.4%,3.3% and 3.6%,respectively.The enrichment factors for the three carboxylic acids were within the range of 8-10 times.The recoveries for the aged oil samples ranged from 91.7%to 107%.The proposed method is simple and effective,and provides analytical data for the correct use of aged characteristic quantity of transformer oil paper insulation and study on effect of carboxylic acid on aged oil paper insulation.
Key Words:silylation derivatization  gas chromatography-tandem mass spectrometry(GC-MS)  short-chain carboxylic acid  dispersive liquid-liquid microextraction(DLLME)  high performance liquid chromatography(HPLC)  transformer oil
引用本文:李海燕,华佳,王逸凡,杨珍,李吟霜.基于BSTFA衍生/GC-MS与DLLME/HPLC的老化变压器油中短碳链羧酸的分析[J].分析测试学报,2019,(4):385-389.
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