高效液相色谱法测定3,4-二氟苯腈和3,4-二氯苯腈  

Determination of 3,4-Difluorobenzonitrile and 3,4-Dichlorobenzonitrile by High Performance Liquid Chromatography

作　　者：沈阳[1] 陈惠[1] 曹旭妮[1] 

机构地区：[1]华东理工大学生物工程学院生物反应器工程国家重点实验室,上海200237

出　　处：《化学试剂》2016年第5期433-436,共4页Chemical Reagents

基　　金：国家自然科学基资金助项目(21375039);上海市科委资助项目(131422009031;14JC1490902)

摘　　要：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210nm，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／mL，线性范围分别为0．1—500和0．1～100μg／mL，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C18SPE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, and it can be synthesized by using 3,4-dichlorobenzonitrile as the starting material via phase transfer catalysis. A method for simultaneous determination of 3 ,g-difluorobenzonitrile and 3,4-dichlo- robenzonitrile in this chemical reaction was established by high performance liquid chromatography （HPLC）. The detection was conducted by a UV detector at 210 nm with 70% methanol solution as the mobile phase on a YMC Hydrosphere-C18 column. The detection limits were 0. 04 and 0. 03 μg/mL, respectively. The linear ranges were 0. 1 - 500 μg/mL and 0. 1 - 100μg/mL, re- spectively. The recoveries were ranged from 92% - 106% , RSD was between 1.0% -2.5%. When 3,4-dichlorobenzonitrile were extracted by C18 SPE column,it were successfully detected at the level of 0. 2% in the self-made product of 3,4-difluorobenzoni- trile,and the recovery was 97%.

关 键 词：3 4-二氯苯腈 3 4-二氟苯腈 高效液相色谱 

分 类 号：O657.7[理学—分析化学]