正相高效液相色谱法测定叔丁基过氧化氢

建立了丙烯环氧化反应中叔丁基过氧化氢(TBHP)的高效液相色谱分析方法。考察了色谱柱类型、流动相配比和检测器紫外吸收波长对测定结果的影响,得到了高效液相色谱法测定TBHP含量的适宜分析条件。即采用Hypersil NH2正相色谱柱(250 mm×4.6 mm×5μm),以体积比80∶20的乙腈-二氯甲烷混合溶液为流动相,流量1.0 mL/min,柱温30℃,紫外检测波长222 nm。测试结果表明,丙烯环氧化反应产物中的组分在4 min内可完全出峰,并得到良好的分离;TBHP质量浓度在0.17～17.30 mg/mL内时,其与峰面积呈现良好的线性关系,相关系数r=0.999 9,检出限为3.46μg/mL,加标回收率达99.4%～101.2%。该分析方法准确、快速且灵敏度较高。

Determination of tert-Butyl Hydroperoxide by Normal Phase High Performance Liquid Chromatography

A normal phase high performance liquid chromatography(HPLC) for the determination of tert-butyl hydroperoxide(TBHP) in a propylene epoxidation system was established.The effects of different chromatographic columns,ratio of acetonitrile to dichloromethane as the mobile phase and UV absorption wavelength of the detector on the HPLC method were investigated.Under the appropriate analysis conditions of Hypersil NH2 normal phase chromatographic column(250 mm×4.6 mm×5 μm),volume ratio of acetonitrile to dichloromethane 80∶20,flowrate of the mobile phase 1.0 mL/min,column temperature 30 ℃ and UV absorption wavelength 222 nm,the TBHP in the propylene epoxidation system could be separated in 4 min and a good linear relationship was showed in the range of 0.17-17.30 mg/mL with a correlation coefficient of 0.999 9.The detection limit is 3.46 μg/mL and the recovery is in the range of 99.4%-101.2%.Compared with gas chromatography,the HPLC method is accurate,rapid and sensitive.