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3,4-二氟苯腈是一种重要的中间体,目前合成方法有采用3,4-二氯苯腈为原料,通相转移催化制备,由此建立了反应过程中同时测定3,4-二氟苯腈和3,4-二氯苯腈的高效液相色谱定量分析方法。以C18色谱柱为分离柱,70%甲醇水溶液为流动相;紫外检测波长设定为210 nm,可以实现反应液中这两种物质的同时检测。3,4-二氟苯腈和3,4-二氯苯腈的最低检出浓度分别为0.04和0.03μg/m L,线性范围分别为0.1~500和0.1~100μg/m L,方法的回收率为92%~106%,相对标准偏差(RSD)为1.0%~2.5%。此外,进一步考察C18 SPE小柱富集微量3,4-二氯苯腈的方法,可以实现3,4-二氟苯腈粗品中3,4-二氯苯腈的含量分析,自制的3,4-二氟苯腈样品中,3,4-二氯苯腈的含量为0.2%,加标回收率为97%。
3,4-difluorobenzonitrile is an important intermediate. At present, 3,4-dichlorobenzonitrile is used as a raw material and prepared by phase-transfer catalysis. The simultaneous determination of 3,4 - Difluorobenzonitrile and 3,4-Dichlorobenzonitrile by High Performance Liquid Chromatography Quantitative Analysis Methods. Using C18 column as the separation column and 70% aqueous methanol as mobile phase, UV detection wavelength was set at 210 nm, and simultaneous detection of these two substances in the reaction solution could be achieved. The minimum detectable concentrations of 3,4-difluorobenzonitrile and 3,4-dichlorobenzonitrile were 0.04 and 0.03 μg / mL, respectively, with linear ranges of 0.1 to 500 and 0.1 to 100 μg / mL, respectively. The method recovery Rates ranged from 92% to 106% with relative standard deviations (RSDs) of 1.0% to 2.5%. In addition, further investigation of C18 SPE cartridge enrichment of trace 3,4-dichlorobenzonitrile method can be 3,4-dichlorobenzonitrile content of 3,4-difluorobenzonitrile crude product analysis, homemade 3, In the 4-difluorobenzonitrile sample, the content of 3,4-dichlorobenzonitrile was 0.2% and the recovery rate was 97%.