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Method for controlling quality of alprostadil injection

A technology of alprostadil and prostaglandin, which is applied in the preparation of test samples, measuring devices, instruments, etc., can solve the problems of complex process, inaccurate analysis results, affecting analysis precision and accuracy, etc.

Inactive Publication Date: 2009-11-18
上海万特医药科技(集团)有限公司
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0006] However, in the analysis method adopted by the national drug standard WS1-(X-041)-2002Z, the pretreatment process of the test sample is complicated, and it must first be separated by a C18 column, and then concentrated under reduced pressure
In these two processes, a part of PGE1 and PGA1 will be lost in the C18 column. What is more serious is that PGE1 is significantly degraded in the vacuum distillation, which leads to inaccurate analysis results of PGE1 and PGA1, which seriously affects the analysis. The precision and accuracy of

Method used

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  • Method for controlling quality of alprostadil injection
  • Method for controlling quality of alprostadil injection
  • Method for controlling quality of alprostadil injection

Examples

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preparation example Construction

[0032] Preparation of internal standard solution Take about 25mg of β-naphthol, weigh it accurately, put it in a 50ml measuring bottle, add absolute ethanol to dissolve and dilute to the mark, measure 5ml, put it in a 50ml measuring bottle, add mobile phase to dilute to the mark, Shake well and serve.

[0033] The preparation of reference substance solution gets about 5 mg of alprostadil reference substance (in a phosphorus pentoxide decompression desiccator, dried at room temperature for 4 hours), accurately weighed, puts in a 50ml brown measuring bottle, adds dehydrated alcohol 10ml to dissolve, and Dilute to the mark, shake well, accurately measure 5ml to a 100ml measuring bottle, add mobile phase to dilute to the mark, shake well, accurately measure 1ml and 1ml of internal standard solution, put it in a 10ml measuring bottle, add mobile phase to dilute to the mark, Shake well as a reference solution.

[0034] Preparation of the test solution Precisely measure an appropria...

Embodiment 1

[0041] Prostaglandin A 1 Determination of

[0042] According to high performance liquid chromatography (Chinese Pharmacopoeia 2000 edition two appendix V D) determination.

[0043] 1. Chromatographic conditions

[0044] Instrument: Agilent 1100 HPLC

[0045] Chromatographic column: Kromasil C18, 4.6×250mm, 5μm

[0046] Mobile phase: 0.0067mol / L phosphate buffer: acetonitrile (74:26)

[0047] Flow rate: 1.4ml / min

[0048] Post-column reaction equipment: Waters 515 pump, Waters column thermostat

[0049] Post-column reaction solution: 1mol / L potassium hydroxide solution

[0050] Post-column reaction tube: polytetrafluoroethylene tube (φ0.5mm×10m)

[0051] Column temperature: 60°C Detection wavelength: 278nm Injection volume: 100μl

[0052] Flow rate: 0.3ml / min

[0053] 2. Reagent and test solution

[0054] Alprostadil reference substance (National Institute for the Control of Pharmaceutical and Biological Products)

[0055] Alprostadil raw material (raw material when ma...

Embodiment 2

[0102] Determination of PGE1 content

[0103] According to high performance liquid chromatography (Chinese Pharmacopoeia 2000 edition two appendix V D) determination. After system suitability test, precision test, linear regression test and recovery rate test, the results are satisfactory.

[0104] 1. Chromatographic conditions: the same as the detection method of prostaglandin A1 in Example 1

[0105] 2. System suitability test See the system suitability test under the item of prostaglandin A1 in Example 1.

[0106] 3. Precision test

[0107] Prepare according to the sample solution preparation method, repeat the measurement 6 times according to the content determination method, record the ratio of the main peak area to the internal standard peak area, and calculate the relative standard deviation. (See Table 4)

[0108] Table 4 precision test results

[0109]

[0110] Because the RSD<2.0%, the sample precision test results meet the requirements of the Pharmacopoeia m...

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Abstract

The invention discloses a method for measuring prostaglandin E1 and / or prostaglandin A1 in alprostadil fat emulsion injection, which comprises the following steps: (1) ultrasonically processing the alprostadil fat emulsion injection, obtaining an alprostadil solution of which the fat phase is removed; and (2) performing high performance liquid chromatography measurement to the alprostadil solution of which the fat phase is removed, obtaining the content of the prostaglandin E1 and / or prostaglandin A1, wherein the conditions of the high performance liquid chromatography measurement are as follows: stationary phase: octadecyl ether-bonded monolithic silica is filling agent, mobile phase: the ratio of phosphate buffer to acetonitrile is equal to 1-6:1, and the detection wavelength is 278 nm. The method can accurately measure the alprostadil and the degradation products thereof in the alprostadil fat emulsion injection.

Description

technical field [0001] The invention belongs to the field of pharmaceutical technology, and more specifically relates to a quality control method for alprostadil injection, and relates to an analysis and quality control method for alprostadil and alprostadil related substances in fat microemulsion preparations. Background technique [0002] Alprostadil injection is a preparation in which alprostadil is formed into fat microemulsion by high-pressure homogenization. The chemical name of alprostadil is prostaglandin E1 (abbreviated as PGE1), and PGE1 is very unstable and rapidly decomposes into prostaglandin A1 (abbreviated as PGA1) at room temperature. The biological activity of PGA1 is very low and loses its therapeutic significance. [0003] The original analysis method and quality control have been made public (Chinese National Drug Standard WS1-(X-041)-2002Z). In the standard of this quality control, the method adopted in the content analysis of the degradation substance...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N1/28
Inventor 陈中怡
Owner 上海万特医药科技(集团)有限公司
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