Method for detecting alprostadil freeze-dried lipid emulsion

Abstract

The invention provides a method for detecting an alprostadil freeze-dried lipid emulsion. The method comprises the steps: 1) adding water to the alprostadil freeze-dried lipid emulsion, and re-dissolving to obtain a sample aqueous solution; 2) demulsifying the sample aqueous solution obtained in the step 1) with a demulsifier, to obtain a demulsified sample solution, wherein the volume ratio (ml:ml) of the demulsifier to the sample aqueous solution is 5:1-5:6; and 3) determining the contents of alprostadil and prostaglandin A1 in the demulsified sample solution obtained in the step 2) by high performance liquid chromatography, wherein the demulsifier is composed of an organic solvent A and an organic solvent B, the organic solvent A is selected from the group consisting of alcohols, and the organic solvent B is selected from the group consisting of alkanes or tetrahydrofuran. The method for detecting the alprostadil freeze-dried lipid emulsion has the advantages of high recovery rate and accurate measurement results, enhances quality detection standards of the alprostadil freeze-dried lipid emulsion, reinforces the quality controllability of drugs, thereby ensuring the effectiveness and the safety of clinical medication.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and in particular relates to a method for determining the lyophilized lipid emulsion of alprostadil, which can be used to simultaneously determine the content of the active ingredient alprostadil in the lipid emulsion of alprostadil and the content thereof. Related Substance Prostaglandin A 1 content. Background technique [0002] Alprostadil, aka prostaglandin E 1 , English name Prostaglandins E 1 , English abbreviation PGE 1 , chemical name: 11a, 15(S)-bishydroxy-9-carbonyl-13-reprostenic acid, molecular formula: C 20 h 34 o 5 , the molecular weight is: 354.49, and the structural formula is: [0003] . [0004] Alprostadil is a highly active physiologically active substance that can inhibit platelet aggregation, prevent thromboxane A 2 Forming and inhibiting the formation of atherosclerotic plaques and protecting vascular endothelial cells and other physiological functions; it ...

AI Technical Summary

Problems solved by technology

Due to PGE 1 Unstable under acidic conditions, and the solid-phase extraction process is complex and cumbersome, which is prone to large measurement errors, expensive experimental consumables, inconvenient to use experimental instruments, and the solvent is easily destroyed by evaporating the solvent at 50°C. 1 , to convert it into PGA 1 , causing the true content of the sample to be low and the PGA 1 Too much content

[0008] Chinese patent CN1823786A adopts freeze-drying method to demulsify, the process is complex, time-consuming, high energy consumption, high cost, it is difficult to measure the content of samples, the operability is not strong, and the production process cannot be controlled

And the freeze-drying equipment is rare, and the practicability is not strong

[0009] In the national drug standard YBH01492010 and CN101158665 B patent of alprostadil dry emulsion for injection announced by the State Food and Drug Administration, the sample solution prepared by the demulsification method is obviously stratified and the mass distribution is uneven, which leads to the measured content ratio Significant increase in actual content, poor controllability of content, large measurement error, poor repeatability of measurement results, and extremely poor solution stability

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