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Method for detecting gentamicin C1a as starting material of etimicin

A technology of gentamicin and etimicin, which is applied in the field of chemical analysis, can solve the problems of inability to correspond to impurities, poor separation of impurities, and large gaps, and achieve good specificity and rapid and accurate detection methods

Pending Publication Date: 2022-03-01
CHANGZHOU FANGYUAN PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method can directly calculate the sample purity, but this method is quite different from the finished product method. Derivatization will produce many derivatized peaks, and the separation of impurities is poor. It cannot correspond to the impurities in the finished product one by one, and the quality of the finished product cannot be well controlled.

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  • Method for detecting gentamicin C1a as starting material of etimicin

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Experimental program
Comparison scheme
Effect test

Embodiment 1）

[0028] The present embodiment detects the gentamycin C in the etimicin desorption solution 1a , directly detected without preprocessing.

[0029] Chromatographic conditions: packing particle size 5μm, column size 150mm×6.6mm.

[0030] In the mobile phase, acetonitrile:0.01M trifluoroacetic acid=35:65; flow rate 0.5mL / min.

[0031] The injection volume is 10 μL.

[0032] The derivatization reagent of this embodiment: Weigh 10 g of boric acid, 5 g of sodium hydroxide, add 800 mL of water to dissolve; weigh 200 mg of o-phthalaldehyde, dissolve with 10 mL of methanol, add the o-phthalaldehyde solution into the boric acid buffer solution, and dilute with water to 1L, then add 0.5mL of thioglycolic acid, mix well for later use, and prepare immediately for use.

[0033] Derivatization conditions: the flow rate of the derivatization reagent is 0.5 mL / min, and the derivatization reaction temperature is 45°C.

[0034] The detection wavelength is 330nm.

[0035] The specificity map ...

Embodiment 2）

[0038] Gentamicin C of the present embodiment 1a The detection method all the other are identical with embodiment 1, difference is:

[0039] Chromatographic conditions: packing particle size 4μm, column size 150mm×5mm.

[0040] In the mobile phase, acetonitrile:0.01M trifluoroacetic acid=30:70; flow rate 0.5mL / min.

[0041] The injection volume is 10 μL.

[0042] Derivatization conditions: the flow rate of the derivatization reagent is 0.5 mL / min, and the derivatization reaction temperature is 50°C.

[0043] The detection wavelength is 335nm.

[0044] Test result: Gentamicin C 1a The main impurities in the test substance and the main impurity were all achieved baseline separation.

Embodiment 3）

[0046] Gentamicin C of the present embodiment 1a The detection method all the other are identical with embodiment 1, difference is:

[0047] Chromatographic conditions: packing particle size 6μm, column size 250mm×6.6mm.

[0048] In the mobile phase, methanol:0.02M trifluoroacetic acid=20:80; flow rate 1.0mL / min.

[0049] The injection volume is 20 μL.

[0050] Derivatization conditions: the flow rate of the derivatization reagent is 1.0 mL / min, and the derivatization reaction temperature is 65°C.

[0051] The detection wavelength is 350nm.

[0052] Test result: Gentamicin C 1a The main impurities in the test substance and the main impurity were all achieved baseline separation.

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Abstract

The invention discloses a method for detecting gentamicin C1a serving as a starting material of etimicin, which adopts a post-column derivatization method and comprises the following steps: separating a to-be-detected sample containing gentamicin C1a through an HPLC (High Performance Liquid Chromatography) chromatographic column, carrying out derivatization reaction after separation, and detecting the obtained derivative in an ultraviolet-visible light detector; wherein the chromatographic conditions are as follows: a mobile phase A is methanol or acetonitrile, and a mobile phase B is 0.01-0.03 M trifluoroacetic acid; the volume ratio of the mobile phase A to the mobile phase B is (35-5): (65-95), and the flow velocity is 0.5-1.0 mL / min; the derivatization reagent is an o-phthalaldehyde solution, the flow velocity of the derivatization reagent is 0.5-1.0 mL / min, and the derivatization reaction temperature is 40-70 DEG C. The detection method is rapid and accurate, and the purity and content of gentamicin C1a in a sample can be detected on line by using a conventional ultraviolet-visible light detector and a high performance liquid chromatograph.

Description

technical field [0001] The invention relates to the technical field of chemical analysis, in particular to a kind of etimicin starting material gentamicin C 1a detection method. Background technique [0002] Gentamicin C 1a It is the starting material of etimicin. Such as Chinese patent CN1040177C (application number: 93112412.3) discloses a kind of containing 1-N-ethyl gentamicin C 1a The preparation method and medicinal preparation of its salt, the preparation method of 1-N-ethyl gentamycin C1a is as follows: the first step, the gentamycin C of purification 1a Dissolve in water or aprotic organic solvents (such as N,N-dimethylformamide, dimethyl sulfoxide, etc.) at room temperature, then add cobalt acetate, dropwise add the tetrahydrofuran solution of acetic anhydride, and keep warm until the reaction is complete , and then purified and concentrated by 732 strong acidic cationic resin column to obtain 3,2', 6'-tri-N-acetyl gentamycin C1a (P1); in the second step, the 3...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/74
CPCG01N30/02G01N30/06G01N30/74G01N2030/067
Inventor 雷翔霄苏晓春杨陈耿贺贺张贾亮
Owner CHANGZHOU FANGYUAN PHARMA
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