CAJ | 학술논문

目的：：参考《欧洲药典》的HPLC-脉冲安培电化学法建立高效液相色谱-柱后衍生化法测定庆大霉素C组分含量及其有关物质,同时与电化学法进行比较研究。方法：采用亲水性Hydrosphere C18(250 mm ×4.6 mm,5μm)色谱柱,以含0.7%三氟乙酸及0.025%五氟丙酸的50 mmol·L-1氢氧化钠溶液(pH 2.6)-乙腈(98.5∶1.5)为流动相。衍生化法反应温度30℃,荧光激发波长340 nm,发射波长430 nm。电化学法采用脉冲安培检测器,金电极为工作电极,四电位波形工作模式。结果：两种方法测定的庆大霉素C组分(C1a, C2, C2a和C1)分别在5.82~233.00,6.92~277.00,4.00~160.00和6.23~249.00μg· ml-1的浓度范围内线性关系良好(r均≥0.9993),检测限和定量限范围分别为0.92~3.28 ng和1.37~5.19 ng。结论：两种方法的检测结果无明显差异。
목적：：삼고《구주약전》적HPLC-맥충안배전화학법건립고효액상색보-주후연생화법측정경대매소C조분함량급기유관물질,동시여전화학법진행비교연구。방법：채용친수성Hydrosphere C18(250 mm ×4.6 mm,5μm)색보주,이함0.7%삼불을산급0.025%오불병산적50 mmol·L-1경양화납용액(pH 2.6)-을정(98.5∶1.5)위류동상。연생화법반응온도30℃,형광격발파장340 nm,발사파장430 nm。전화학법채용맥충안배검측기,금전겁위공작전겁,사전위파형공작모식。결과：량충방법측정적경대매소C조분(C1a, C2, C2a화C1)분별재5.82~233.00,6.92~277.00,4.00~160.00화6.23~249.00μg· ml-1적농도범위내선성관계량호(r균≥0.9993),검측한화정량한범위분별위0.92~3.28 ng화1.37~5.19 ng。결론：량충방법적검측결과무명현차이。
Objective:To establish an HPLC coupled with post column derivatization method for the determination of gentamicin C components and the related substances based on the latest European Pharmacopeia and compare with the electrochemical method. Methods:A Hydrophilic C18(250 mm ×4.6 mm, 5 μm)column was used with acetonitrile-50 mmol·L-1 sodium hydroxide solution ( pH 2. 6) containing 0. 7% trifluoroacetic acid and 0. 025% pentafluoropropanoic acid (1. 5∶98. 5) as the mobile phase. The temper-ature of post-column reaction was set at 30℃, and the samples were detected by a fluorescence detector withλex of 340nm andλem of 430nm. A pulsed amperometric detector (PAD) was applied in the electrochemical method with golden working electrode in a four-po-tential working mode. Results: According to the results of the two detection methods, the linear range of C1a , C2 , C2a and C1 was 5.82-233.00,6.92-277.00,4.00-160.00and6.23-249.00 μg·ml-1(r >0.9993) , respectively. The limit of detection and quantization were 0. 92-3. 28ng and 1. 37-5. 19ng, respectively. Conclusion:There is no significant difference between the determina-tion results of the two methods.