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Method for detecting aminolevulinic acid related substances

A technique for the detection of aminolevulinic acid hydrochloride, which is applied in the field of pharmaceutical analysis, can solve problems such as chromatographic peak shoulders, the number of detected impurities is small, and solvent peaks cannot be effectively separated, achieving good specificity and high detection sensitivity , Improve the effect of product quality control level

Pending Publication Date: 2022-04-01
上海复旦张江生物医药股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the following defects: (1) aminolevulinic acid hydrochloride cannot be retained in the reversed-phase system due to its great polarity, so the main peak appears at the dead volume of the chromatographic column, and cannot be effectively separated from the solvent peak. Sample solution, the chromatographic peak has a shoulder phenomenon
(2) The number of impurities detected is small, and only pyrazine 2,5-dipropionate (impurity A) and pyrazine 3-(4'-carbonylvaleric acid)-2,5-dipropionate ( Impurity B) These two main impurities, the remaining impurities cannot be detected or located, and there are even unidentified impurities

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  • Method for detecting aminolevulinic acid related substances
  • Method for detecting aminolevulinic acid related substances
  • Method for detecting aminolevulinic acid related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～ Embodiment 10

[0046] (1) Experimental equipment and reagents

[0047] Instrument: Agilent HPLC 1260 Method Scouting system

[0048] (2) Chromatographic conditions:

[0049] Chromatographic column: Octadecylsilane bonded silica gel is used as the filler of the chromatographic column, Agilent Zorbax C18 4.6×250mm 5μm. As shown in Table 1 below, it is the chromatographic conditions of Examples 1-10.

[0050] Table 1: Chromatographic conditions of Examples 1-10

[0051]

[0052] Note: mM is the abbreviation of concentration unit mmol / L, 1mM=1×103mol / L.

[0053] (3) Sample preparation: prepare sodium octane sulfonate buffer solution and mobile phase according to the proportioning in Table 2, and then take an appropriate amount of ammonium levulinic acid hydrochloride crude drug, and use mobile phase to prepare it into a solution with a concentration of 10 mg / ml .

[0054] (4) Experimental results:

[0055] Carry out chromatographic separation to embodiment 1~10 respectively, the chromat...

Embodiment 11

[0063] (1) Experimental equipment and reagents

[0064] Instrument: the same as in Examples 1 to 10

[0065] (2) Chromatographic conditions:

[0066] Chromatographic column: with embodiment 1~10

[0067] Flow rate: 1.0ml / min

[0068] Detection wavelength: 205nm

[0069] Column temperature: 30°C

[0070] Injection volume: 20μL

[0071] Mobile phase: sodium octane sulfonate buffer-acetonitrile=86:14 (v / v) (the preparation of sodium octane sulfonate buffer is as follows: get sodium octane sulfonate 4.75g (20mM), ammonium dihydrogen phosphate 7.59 g (66mM), add 980ml of water to dissolve, adjust the pH value to 1.90 with phosphoric acid, and add water to dilute to 1000ml).

[0072] (3) Sample preparation: Weigh an appropriate amount of levulinic acid hydrochloride preparation containing auxiliary materials and auxiliary material degradation impurities (p-hydroxybenzoic acid), and use mobile phase to prepare it into a solution with a concentration of 10 mg / ml.

[0073] (4) E...

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Abstract

The invention provides a method for detecting related substances of aminolevulinic acid hydrochloride, which is a reversed-phase high-performance liquid chromatography and comprises the following steps: preparing a sodium octanesulfonate buffer solution with the pH value of 2.0 + / -0.2, further preparing a sodium octanesulfonate buffer solution-acetonitrile in which the acetonitrile accounts for 10%-20% (v / v) as a mobile phase, and detecting a to-be-detected sample which takes aminolevulinic acid hydrochloride as a main component by using a high-performance liquid chromatography method to obtain the related substances of the aminolevulinic acid hydrochloride. The method comprises the following steps: preparing a test solution with the concentration of 10mg / ml by using the mobile phase, putting 1ml of the test solution into a 20ml measuring flask, diluting to the scale by using the mobile phase, uniformly shaking, and preparing a reference solution for detection operation. The detection method for the aminolevulinic acid hydrochloride related substances is good in specificity and high in detection sensitivity for the related substances, impurity peaks and main peaks can be completely separated, more substance types can be detected, four impurities generated in the degradation process of aminolevulinic acid hydrochloride can be identified, and the detection method is suitable for large-scale industrial production. And two of the two substances are new substances which are never identified before.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular to a method for detecting related substances of aminolevulinic acid hydrochloride. Background technique [0002] Aminolevulinic Acid Hydrochloride (Aminolevulinic Acid Hydrochloride), its chemical name is 5-amino-4-ketopentene hydrochloride, molecular formula: C 5 h 9 NO 3 • HCl, molecular weight: 167.59. Aminolevulinic acid (ALA) metabolism is the first step in the biochemical pathway for heme synthesis in humans. ALA itself is not a photosensitizer, but rather a metabolic precursor of the photosensitizer protoporphyrin IX (PpIX). ALA synthesis is normally regulated by intracellular heme levels through feedback inhibition of ALA synthase. Exogenous ALA circumvents this regulation, leading to the accumulation of PpIX. Photosensitivity after skin application of aminolevulinic acid hydrochloride due to conversion of ALA to PpIX and accumulation. When exposed to light of a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/86
Inventor 薛逸君蒋剑平陈毓婷
Owner 上海复旦张江生物医药股份有限公司