高效液相色谱法分析间二异丙苯的氧化产物

建立了用高效液相色谱(HPLC)分析间二异丙苯(DIPB)氧化制备间苯二酚反应的中间产物的方法;考察了HPLC条件对分析结果的影响,得到了最佳HPLC条件;同时在该HPLC条件下定性、定量分析了DIPB氧化产物的组成。实验结果表明,标准物DIPB、1,3-二苄醇二异丙苯(DCL)和1,3-二苯乙酮(DAC)的标准工作曲线的线性关系很好,相关系数为0.99804～0.99952;最佳HPLC条件为:采用InertsilSIL-100A色谱柱(5μm×4.6mm×250mm),以V(正己烷):V(异丙醇)=95:5的混合液为流动相,流动相的流量1.0mL/min,紫外检测波长257nm,柱温(30±2)℃,进样量3μL;在此条件下,DIPB,DCL,DAC分析结果的平均误差均小于1.00%,相对标准偏差为0.09%～0.25%,回收率为97.41%～103.96%,DIPB氧化产物分离效果好,分析时间短,定性、定量分析结果较为准确。

Analysis of m-Diisopropylbenzene Oxidation Products by High Performance Liquid Chromatography

Analytical method for separating and determinating the products of m-diisopropylbenzene(DIPB) oxidation in synthesis of resorcinol were established by means of high performance liquid chromatography(HPLC).The main objects of analysis were DIPB,1,3-dihydroperoxide diisopropylbenzene,1-(2-hydroperoxy-2-propyl)-3-(2-hydroxy-2-propyl) benzene,1,3-di(2-hydroxy-2-propyl)benzene(DCL),3-(2-hydroperoxy-2-propyl)isopropylbenzene,3-(2-hydroxy-2-propyl)isopropylbenzene,3-isopropyl acetophenone,3-(2-hydroperoxy-2-propyl) acetophenone and 3-(2-hydroxy-2-propyl)acetophenone.The results indicated good linear correlation of standard working curves of DIPB,DCL and 1,3-diacetophenone(DAC).Linear regression coefficients are from 0.998 04 to 0.999 52.Under the conditions of Inertsil SIL-100 A chromatographic column(5 μ m×4.6 mm×250 mm),hexane-isopropyl alcohol mixture as mobile phase(volume ratio 95:5),flow rate 1.0 mL/min at(30±2)℃,UV detection at wavelength 257 nm,sample capacity 3 μ L,for DIPB,DCL and DAC the recovery rates were in the range of 97%-104% with relative standard deviations 0.09%-0.25% and average error less than 1.00%.Under the above conditions the products are separated satisfactorily with relatively short operation time and precise analytical results.