Novel method for detecting etimicin sulfate

Abstract

The invention relates to a method for detecting the content of an etimicin sulfate raw material and preparation of the etimicin sulfate raw material and relevant substances. The method adopts precolumn derivatization, the derivatization condition comprises taking 4ml sample with appropriate concentration, adding 1ml O phthalic aldehyde (OPA) solution into the sample, diluting the mixed solution with isopropyl alcohol to 10ml, heating the mixed solution at 30-60 DEG C in water bath away from light, and obtaining derivatization solution. The novel method for detecting etimicin sulfate adopts a high efficiency liquid chromatograph, the chromatographic condition is that an octadecylsilane chemically bonded silica filler chromatographic column has particle size ranging from 4-10mum, column specification is 150-250mmX4.6-8.0mm; flowing phase is divided into organic phase and aqueous phase, wherein the volume rate of the organic phase to the aqueous phase is 55-75:45-25, the organic phase is methyl alcohol or acetonitrile, the aqueous phase is glacial acetic acid containing 0.01M-0.03M ion pair reagent sodium heptanesulfonate, potential of hydrogen (PH) range is adjusted by ammonia water or ammonium acetate; flow speed is 0.5-1.0ml / min; sample feeding amount is 10-20mul; a detector is a conventional ultraviolet-visible light detector, and detection wavelength is from 330-350nm. The novel method for detecting etimicin sulfate adopts the conventional detector and the high efficiency liquid chromatograph, can achieve on-line detection of the content of the etimicin sulfate, the preparation of the etimicin sulfate and the relevant substances, and is simple, convenient, feasible, accurate and reliable.

Description

technical field [0001] The present invention relates to a high-performance liquid chromatography analysis method, in particular to a method based on pre-column derivatization, using octadecylsilane bonded silica gel as a separation filler to determine the content of etimicin sulfate and its preparations and related substances analysis method. Background technique [0002] Etimicin sulfate is a semi-synthetic aminoglycoside antibiotic independently developed in my country with independent intellectual property rights. It is widely used in clinical practice because of its broad antibacterial spectrum, low ear and kidney toxicity, and low drug resistance. For a long time, etimicin sulfate has only the ultraviolet absorption terminal absorption and is difficult to measure with ultraviolet detectors, so the content and related substances can only be determined by methods such as biological potency method and optical rotation method. These methods are cumbersome to operate and ha...

AI Technical Summary

Problems solved by technology

For a long time, etimicin sulfate is difficult to measure with ultraviolet detector because it only absorbs at the end of ultraviolet absorption, so the content and related substances can only be determined by methods such as biological potency method and optical rotation method.

These methods are cumbersome to operate and have low accuracy and reliability

There are some studies on the content determination of etimicin sulfate with general-purpose detectors at present. Although general-purpose detectors such as differential refractive index detectors and evaporative light scattering detectors have advantages in the determination of etimicin content, due to their sensitivity Low specificity and poor reproducibility often fail to achieve satisfactory results in the determination of etimicin related substances, and controlling the amount of related substances is the key to the quality control of etimicin sulfate

It has also been reported in the literature that pre-column derivatization was used to determine aminoglycoside antibiotics, but the resolution did not meet the requirements, the derivatization reagents were also different, and the derivatization efficiency was low