摘要
建立了变压器油中糠醛及呋喃类化合物(5-羟甲基糠醛、2-呋喃甲醇、糠醛、2-乙酰呋喃和5-甲基-2-呋喃)的高效液相色谱分析方法。样品经固相萃取小柱(SPE)富集后,用乙腈-水混合溶剂从柱上洗脱糠醛及呋喃类化合物。采用AgilentC18柱为固定相,乙腈-水混合溶液为流动相进行分离,在二极管列阵检测器(DAD)波长为280nm和217nm处测定。5-羟甲基糠醛、2-呋喃甲醇、糠醛、2-乙酰呋喃和5-甲基-2-呋喃等5种呋喃化合物质量浓度在0.1mg/L^5.0mg/L范围内与其峰面积呈线性关系,检出限(3S/N)分别为0.01mg/L、0.02mg/L、0.01mg/L、0.01mg/L和0.02mg/L。5种组分的平均回收率83%~96%,相对标准偏差RSD均小于3%。本方法适用于变压器油样中糠醛及呋喃类化合物5种组分的检测。
An analytical method of high performance liquid chromatography(HPLC) has been developed for the determination of 2-Furaldehyde and related furanic compounds (5-Hydroxymethyl-2- furaldehyde, 2-Furfuryl alcohol, 2-Furaldehyde, 2-Acetylfuran and 5-Methyl-2-furaldehyde) in transformer oil. The sample was taken and passed through the SPE column to enrich trace amount of these five furanic compounds on the column, and extracted with water-acetone mixture. The extract was separated on Agilent C18 column using a mixture of water and acetonitrile as mobile phase, and determined with Diode Array Detector at the wavelengths of 280nm and 217nm. Linear relationship between values of peak area and mass concentration of these five furanic compounds was obtained in the range of 0.1-5.0 mg/L, with detection limit ( 3S/N ) of 0.01 rag/L, 0.02 mg/L, 0.01 mg/L, 0.01 mg/L and 0.02 rag/L, the average recoveries fonrl 83%-96% and the RSD less than 3.0%. These experimental results demonstrate that five furanic compounds in transformer oil samples can be determined with the new method for practical uses.
出处
《上海计量测试》
2012年第1期18-21,共4页
Shanghai Measurement and Testing
关键词
变压器油
糠醛
呋喃类化合物
固相萃取
高效液相色谱法
transformer oil
2-Furaldehyde
furanic compounds
solidphase extraction (SPE)
high performance liquid chromatography (HPLC)