高效液相色谱法测定植物绝缘油中抗氧化剂含量

Antioxidants Content in Vegetable Insulating Oil Determined by HPLC

采用高效液相色谱法（HPLC）测定植物绝缘油中抗氧化剂的含量,将待测油样与甲醇混合振荡,经过两次离心萃取,合并上层清液用甲醇定容;萃取液经0.45μm滤膜过滤后进入色谱柱分析,以超纯水-甲醇为流动相,采用紫外分光检测器,根据保留时间进行定性分析,根据峰面积进行定量检测。在测定条件下,浓度范围为0.1~0.5 mg/m L的3种抗氧化剂（PG、BHA、BHT）都具有较好的线性关系,相关系数R2大于0.999,检出限为0.003~0.01 mg/m L,定量下限为0.01~0.033 mg/m L;空白样品的加标回收率为98%~108%,相对标准偏差均低于4%。将本方法用于库柏油FR3中抗氧化剂的检测和加标回收试验,结果准确,回收率高。

The high performance liquid chromatography（HPLC） was used to measure the antioxidants content in vegetable insulating oil. The oil samples were mixed with methanol by oscillation, then the supernatant was diluted with methanol after two times of centrifugal extraction. The extract, after filtering by 0.45 μm membrane, was analyzed by UV detector using ultrapure water-methanol as mobile phase.The qualitative analysis was based on retention time, and the quantitative detection was based on peak area. Three antioxidants（PG, BHA, BHT）, whose concentrations ranged from 0.1mg/m L to 0.5mg/m L, had good linear relationship, and the correlation coefficients（R2） was larger than 0.999. The limits of determination（LOD） ranged from 0.003 mg/m L to 0.01mg/m L, and the limits of quantization（LOQ） ranged from 0.01 mg/m L to 0.033 mg/m L. The adding standard recovery of blank sample ranged from 98% to108%, and the relative standard deviation（RSD） was less than 4%. The method was successfully applied in the determination of antioxidant content in the FR3 and the recovery test, and the results are accurate with high recovery rate.