摘要
目的:建立柱前衍生化高效液相色谱法测定氯霉素滴眼液中的二氯乙酸。方法:用2-硝基苯肼盐酸盐对样品进行衍生化,HPLC法进行测定:色谱柱为Diamonsil Plus C_(18)柱(250 mm×4.6 mm,5μm),以0.1%磷酸溶液-乙腈为流动相进行梯度洗脱,流速为1.0 ml·min^(-1),进样量为20μl,柱温为35℃,检测波长为389 nm。结果:衍生化产物在5 h内稳定,在80.1~1067.6 ng·ml^(-1)范围内线性关系良好(r=0.9994),检测限为27 ng·ml^(-1),平均加样回收率为101.5%(RSD=3.7%,n=9)。结论:本法专属性好,灵敏度高,准确可靠,可用于氯霉素滴眼液中二氯乙酸的测定。
Objective:To establish a pre-column derivatization HPLC method for the determination of dichloroacetic acid in chloramphenicol eye drops.Methods:After dichloroacetic acid was derivatized by 2-nitrophenylhydrazaine hydrochloride(2-NPH·HCl),HPLC was performed on a Diamonsil Plus C_(18)(250 mm×4.6 mm,5μm)column with gradient elution of 0.1%phosphoric acid solution-acetonitrile at the flow rate of 1.0 ml·min^(-1).The injection volume was 20μl and the temperature was 35℃.The detection wavelength was set at 389 nm.Results:The derivative kept stable in 5 hours.The calibration curve was linear within the range of(80.1-1067.6)ng·ml^(-1)(r=0.9994).The limit of detection(LOD)was 27 ng·ml^(-1) and the average recovery was 101.5%(RSD=3.7%,n=9).Conclusion:The method is sensitive and accurate,and can be used for the determination of dichloroacetic acid in chloramphenicol eye drops.
作者
徐然
李丹
邓思维
邵冉薇
Xu Ran;Li Dan;Deng Siwei;Shao Ranwei(Nanjing Institute for Food and Drug Control,Nanjing 211198,China)
出处
《中国药师》
CAS
2022年第10期1811-1814,共4页
China Pharmacist
基金
南京市市场监督管理局科技项目(编号:Kj2020046)。
