Method for analyzing etimicin

Abstract

The invention relates to a method for detecting etimicin and related substances thereof. The method adopts high performance liquid chromatography; chromatographic conditions are that: polystyrene-divinylbenzene polymer chromatographic column is MKF-RP-ETI (the particle size is between 4 and 10mu m, the column specification is (100-300)*(8.0-4.6)mm (I.D.)); the volume ratio of compositions of a mobile phase is that the volume ratio of an acetate buffer solution (the pH value is between 4 and 7) with a concentration of between 0.10 and 0.50mol / L to acetonitrile is 90-100: 10-0; the flow rate is between 0.8 and 1.2mL / min; a detector is a refractive index detector; and the injection volume is between 10 and 20muL. The method can finish the on-line detection on the etimicin and the related substances by using the prior HPLC instrument and refractive index detector; and the method is simple, quick and accurate.

Description

(1) Technical field [0001] The invention relates to a high-performance liquid chromatography (HPLC) detection method, in particular to an analysis method for content determination of etimicin and its related substances using a polystyrene-divinylbenzene chromatographic medium as a separation carrier. (2) Background technology [0002] Etimicin sulfate (etimicin) is a national first-class new drug, and it is a new generation of semi-synthetic aminoglycoside antibiotics with independent intellectual property rights researched and developed by Chinese scientific and technological personnel. As a new drug, its quality control and safety evaluation are particularly important. At present, the methods for determining the content of etimicin mainly include microbial method, optical rotation method, and HPLC method. Among them, the microbial method is cumbersome to operate and has large errors. This method has been eliminated in the determination of etimicin content in the 2005 edit...

AI Technical Summary

Problems solved by technology

Among them, the microbial method is cumbersome to operate and has large errors. This method has been eliminated in the determination of etimicin content in the 2005 edition of the Chinese Pharmacopoeia; while the optical rotation method has poor accuracy and low repeatability; relatively speaking, the HPLC method has high sensitivity and good accuracy. However, etimicin only has ultraviolet terminal absorption, and it is difficult to directly measure it with a UV detector. Usually, the sample needs to be subjected to pre-column derivatization treatment, or other general-purpose detectors, such as evaporative light scattering detectors (ELSD), etc. [See: Wang Mingjuan, Hu Changqin, Jin Shaohong, Chinese Journal of Clinical Medicine, 2004, 5(6): 4-6; National Pharmacopoeia Commission, Pharmacopoeia of the People's Republic of China, 2005 edition, Beijing: Chemical Industry Press, 2005, 730]

Among them, the pre-column derivatization reagent method is cumbersome, time-consuming, and has many influencing factors, and some by-products may be produced during the reaction process, which interferes with the inspection of related substances or purity analysis [see: Zhang Mei, Yuan Yaozuo, Fan Qingfeng, Experiment and Research , 2004, 28(7): 314~316]; the 2005 edition of the Chinese Pharmacopoeia adopts the evaporative light scattering method, which has good specificity, high sensitivity, and meets the detection requirements of drugs, but the ELSD detector used is not suitable for the purification of etimicin. In terms of online detection in the process, the cost is high and the operation is cumbersome, and the purity is falsely high