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Method for separating and measuring lysophosphatidylcholine in drug preparations

A technology for phosphatidylcholine and pharmaceutical preparations, applied in the field of drug analysis, can solve the problems of inability to achieve separation of lysophosphatidylcholine, influence of HPLC column performance, inability to separate samples of injections, etc., so as to ensure drug quality and good separation. , the effect of the simple method

Active Publication Date: 2018-04-24
SHANGHAI JINGFENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing similar detection methods are still unable to separate the injection samples well and achieve limit control
[0003] CN107085061A discloses a method for absolute quantitative analysis of lysophosphatidylcholine based on an HPLC-MS / MS detection platform. The method establishes an HPLC-MS / MS detection platform, and draws LPC14:0-LPC18 with reserpine as an internal standard :0 series substance detection standard curve, and detection of serum matrix effect, the HPLC-MS / MS detection platform for the detection of LPC substances in human serum has high stability and accuracy, to meet clinical needs, but this method can not be achieved Separation of lysophosphatidylcholine from other substances while detecting
[0004] Liu Wenyi et al. (HPLC-ELSD determination of lysophosphatidylcholine content in hydroxycamptothecin liposomes for injection, Strait Pharmacy, Volume 21, No. 8, 2009, pages 37-40) using HPLC-ELSD assay method Determination of the content of lysophosphatidylcholine in hydroxycamptothecin liposomes for injection, select mobile phase A to be methyl alcohol: chloroform (97:3), B is 2% oxalic acid-ethanol (16:84), although can realize hemolysis The content determination of phosphatidylcholine, however, the use of such a mobile phase will affect the performance of the HPLC chromatographic column, so that the life of the chromatographic column is significantly shortened, and the cost is high

Method used

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  • Method for separating and measuring lysophosphatidylcholine in drug preparations
  • Method for separating and measuring lysophosphatidylcholine in drug preparations
  • Method for separating and measuring lysophosphatidylcholine in drug preparations

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Separation and determination of lysophosphatidylcholine in injection by liquid chromatography, the steps are as follows:

[0033] 1. Blank solution: diluent

[0034] 2. Preparation of blank excipient solution:

[0035] Take 1mL of blank injection solution (without egg yolk lecithin), put it in a 10mL measuring bottle, add diluent to dilute to the mark, shake well, and use it as the blank sample solution.

[0036] 3. Preparation of system suitability solution:

[0037] Weigh an appropriate amount of egg yolk lecithin and lysophosphatidylcholine standard substance, add methanol to dilute into a mixed solution containing about 1.2mg of phosphatidylcholine and 0.09mg of lysophosphatidylcholine per 1mL, as the system adaptability of lysophosphatidylcholine solution.

[0038] 4. Preparation of reference solution:

[0039] Accurately weigh an appropriate amount of lysophosphatidylcholine reference substance, add diluent to dissolve to make a solution containing 0.9mg per 1...

Embodiment 2

[0051] Example 2 Recovery test

[0052] Preparation of recovery solution:

[0053] Recovery rate solution: Accurately measure 1ml of alprostadil injection sample, put it in a 10ml measuring bottle, add lysophosphatidylcholine solution equivalent to 80%, 100%, 120% of the limit, add diluent to dilute to the scale, shake well , as the recovery solution. Three replicates were prepared for each concentration.

[0054] Accurately measure 20 μL of the three different concentrations of recovery solutions prepared above, inject them into a liquid chromatograph, use the mobile phase and chromatographic conditions in Example 1, and record the chromatograms.

[0055] According to the measured peak area, the recovery rate of lysophosphatidylcholine was calculated, and the recovery data analysis results are shown in Table 1.

[0056] Table 1

[0057]

[0058] Result analysis:

[0059] According to experimental result (seeing table 1), it can be known that the liquid chromatograph...

Embodiment 3

[0061] The only difference from Example 1 is that the mobile phase is anhydrous methanol-absolute ethanol-glacial acetic acid (500:300:25), and the pH value is adjusted to 6.4 with triethylamine.

[0062] The chromatographic conditions are: flow rate: 1.2 mL / min; column temperature: 30° C.; injection volume: 10 μL; running time: 20 minutes; detector: evaporative photodetector.

[0063] Table 2 Comparison of lysophosphatidylcholine content

[0064]

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Abstract

The invention provides a method for separating and measuring lysophosphatidylcholine in drug preparations. According to the method, a high performance liquid chromatograph is combined with an evaporative light scattering detector to separate and detect drug preparation samples to be detected. When the drug preparation samples to be detected are separated and measured by the high performance liquidchromatograph, a flowing phase is absolute methanol-absolute ethyl alcohol-glacial acetic acid, the volume ratio of the absolute methanol, the absolute ethyl alcohol to the glacial acetic acid is (300-800):(300-800):(15-25), and a pH (potential of hydrogen) value is adjusted to reach 5.6-6.4. The method is simple, efficient, high in accuracy and good in repeatability, good separation can be achieved, separation degree is larger than 1.5, performance of a chromatographic column of the HPLC (high performance liquid chromatograph) cannot be affected, the service life of the chromatographic column cannot be obviously shortened, and the content of lysophosphatidylcholine in drug preparations to be detected can be effectively monitored and controlled, so that drug quality can be effectively guaranteed.

Description

technical field [0001] The invention belongs to the field of drug analysis, and relates to a method for separating and measuring lysophosphatidylcholine in drug preparations. Background technique [0002] Alprostadil injection is produced from Alprostadil, soybean oil, lecithin, glycerin and other auxiliary materials through a specific process. Wherein lecithin is used as an emulsifier, and lysophosphatidylcholine (LPC) is used as an inherent impurity of lecithin. If the content in the injection is too high, it will cause adverse effects on human health. According to the concept of drug QBD quality by design, it is necessary to carry out quality control. However, the existing similar detection methods are still unable to separate the injection samples well and achieve limit control. [0003] CN107085061A discloses a method for absolute quantitative analysis of lysophosphatidylcholine based on an HPLC-MS / MS detection platform. The method establishes an HPLC-MS / MS detection ...

Claims

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88
Inventor 邱永锋杨帅兵薛井中
Owner SHANGHAI JINGFENG PHARMA
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