高效液相色谱法测定对氟苯胺的有关物质  

Determination of Related Substances of p-Fluoroaniline by HPLC

作　　者：张均平 董祥冬 罗恒真 欧阳婷 Zhang Junping;Dong Xiangdong;Luo Hengzhen;Ouyang Ting(Drug R&D Center of Jiangxi Qingfeng Pharmaceutical Co.,Ltd.,Ganzhou 341000,China)

机构地区：[1]江西青峰药业有限公司药物研发中心,江西赣州341000

出　　处：《广东化工》2021年第24期162-165,共4页Guangdong Chemical Industry

摘　　要：目的:建立高效液相色谱法测定对氟苯胺中的苯胺、2-氟苯胺、3-氟苯胺、3,4-二氟苯胺、对氟硝基苯、对氯苯胺、2,4-二氟苯胺。方法:采用Waters Xselect HSS T3为色谱柱(4.6 mm×250 mm×5μm),流动相A为0.01 mol/L磷酸二氢钾溶液(用氢氧化钠溶液调节pH值至6.0),流动相B为乙腈,梯度洗脱;流速为1.0 mL/min;柱温为35℃;检测波长为228 nm;进样体积为20μL。本方法各组分分离度均大于1.5,检测限为0.02μg/mL,检验精密度良好。本方法操作简单,有良好的专属性和灵敏度,可用于对氟苯胺有关物质的检测,对提升对氟苯胺的质量有一定的积极作用。Objective: To establish an HPLC method for the determination of aniline, 2-fluoroaniline, 3-fluoroaniline, 3,4-difluoroaniline, p-fluoronitrobenzene, p-chloroaniline and 2,4-difluoroaniline in p-fluoroaniline. Method: Use Waters Xselect HSS T3 as the chromatographic column(4.6 mm×250 mm×5 μm), mobile phase A is 0.01 mol/L potassium dihydrogen phosphate solution(adjust the pH value to 6.0 with sodium hydroxide solution), and mobile phase B is acetonitrile, gradient elution;Flow rate is 1.0 m L/min;Column temperature is 35 ℃;Detection wavelength is 228 nm;Injection volume is 20 μL. The separation of each component of this method is greater than 1.5, the detection limit is 0.02 μg/mL, and the precision of the test is good. This method is simple to operate, has good specificity and sensitivity, can be used for the detection of p-fluoroaniline related substances, and has a certain positive effect on improving the quality of p-fluoroaniline.

关 键 词：对氟苯胺 高效液相色谱法 有关物质 专属性 灵敏度 

分 类 号：TQ246.31[化学工程—有机化工] O657.72[理学—分析化学]