高效液相色谱法测定3-氯-4-氟苯胺及其有关物质  

Determination of 3-chloro-4-fluoroaniline and its related substances by HPLC

作　　者：王洁 王之羽[1] 石雅丽 WANG Jie;WANG Zhi-yu;SHI Ya-li(Children’s Hospital of Nanjing Medical University,Nanjing 210000,China)

机构地区：[1]南京医科大学附属儿童医院,南京210000

出　　处：《药物分析杂志》2020年第8期1451-1458,共8页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立了测定3-氯-4-氟苯胺及其有关物质的高效液相色谱法。方法:采用Thermo Hypersil GOLD PFP色谱柱(4.6 mm×250 mm,5μm),以乙腈-20 mmol·L^-1磷酸二氢钾水溶液(35∶65)为流动相;检测波长为233 nm。结果:该方法在专属性、线性、精密度、准确性、稳定性和耐用性方面得到了验证。3-氯-4-氟苯胺在0.02~200.0μg·mL^-1范围内线性关系良好(r=1.000),5个有关物质在0.02~100.0μg·mL^-1范围内与峰面积呈现良好线性关系。检测下限和定量下限分别为0.0010~0.1141μg·mL^-1和0.0016~0.0083μg·m L^-1。各杂质的平均回收率在98.4%~107.9%之间,RSD均小于10%(n=9)。结论:本法准确、可靠、灵敏,可用于3-氯-4-氟苯胺及其有关物质测定。Objective:To establish an HPLC method for the determination of 3-chloro-4-fluoroaniline and its related substances. Methods:Separation was achieved on a Thermo Hypersil GOLD PFP column(4.6 mm×250 mm,5 μm). The mobile phase was acetonitrile-20 mmol·L^-1 potassium dihydrogen phosphate acid solution(35∶65),and the detection wavelength was 233 nm. Results:The method was validated in terms of its specificity,linearity,precision,accuracy,stability and ruggedness. The linear relationship of 3-chloro-4-fluoroaniline was good in the range of 0.02-200.0 μg·mL^-1(r=1.000). The correlation coefficients of five impurities were greater than 0.999 in the range of 0.02-100.0 μg·m L^-1. The limits of detection(LODs)and limits of quantificaion(LOQs)were in the range of 0.001 0-0.114 1 μg·mL^-1 and 0.001 6-0.008 3 μg·mL^-1,respectively. The average recovery of each impurity was within 98.4%-107.9%,and the RSD was less than 10%(n=9). Conclusion The method is sensitive and accurate for the determination of 3-chloro-4-fluoroaniline and its related substances.

关 键 词：3-氯-4-氟苯胺 有关物质 基因毒性杂质 高效液相色谱法 方法验证 

分 类 号：R917[医药卫生—药物分析学]