High-efficient liquid-phase chromatographic testing method for copper in aspirin

A technology of high performance liquid chromatography and determination method, which is applied in the field of determination of aspirin copper by high performance liquid chromatography, can solve the problems of aspirin copper decomposition, complex sample components, and increase the difficulty of separation, so as to achieve high solubility, shorten dissolution time, simplify The effect of the compounding process

Inactive Publication Date: 2005-02-23
KUNMING INST OF PRECIOUS METALS
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AI Technical Summary

Problems solved by technology

This analysis method has the following disadvantages: ①Due to the introduction of the internal standard, the sample components are complicated during the analysis process, thus increasing the difficulty of separating the components in the sample
②Due to the low solubility of the sample in acetonitrile and the slow dissolution rate, the sample dissolution process is time-consuming and laborious
③The introduction of phosphoric acid into the mobile phase is helpful for the stability of aspirin copper, but too high or too low acidity will cause the decomposition of aspirin copper, which directly affects whether the separation degree Rs of each component in the sample meets the requirements Rs≥1.5
This brings certain difficulty to the preparation of the mobile phase and is not easy to operate

Method used

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Experimental program
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Effect test

Embodiment Construction

[0017] Instruments and reagents:

[0018] Shimadzu LC-10Avp instrument, Spherisorb C18 column of Dalian Elite Company. Analytical pure methanol, chromatographically pure tetrahydrofuran from Fish Company of the United States, analytically pure aspirin, salicylic acid with a purity >99.5% from Shandong Xinhua Pharmaceutical Factory, analytically pure glacial acetic acid, and secondary deionized water.

[0019] Chromatographic conditions:

[0020] With glacial acetic acid and secondary deionized water as the sample solvent, at 25 °C, C 18 Column (5μm, Φ4.0×250mm), methanol: water: tetrahydrofuran: glacial acetic acid = 45: 52.5: 2.5: 0.5 is the mobile phase, detected under UV-276nm, and the injection volume is controlled within the range of 10-15 μl.

[0021] test methods:

[0022] Take aspirin copper sample 15mg, accurately weighed, use glacial acetic acid and secondary deionized water to settle in a 10ml volumetric flask, and ultrasonically dissolve to obtain the test solut...

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Abstract

A coppr acetylsalicylate high efficient liquid chromatography using liquid phase chromatograph with ultraviolet detector and chromatographic column of octadecylsilane linkage silica gel is featured as using liquid of methanol: water: THF: glacial acetic acid=45:52.5:2.5:0.5 as liquid phase and using 276 mm as detecting wavelength.

Description

technical field [0001] The invention relates to a high-performance liquid chromatography determination method for aspirin copper. Background technique [0002] Chromatographic analysis is often used in drug separation and quantitative analysis research because of its fast, sensitive, and high-resolution characteristics. It is one of the important methods for drug purity analysis and an indispensable method for purity testing required by the Pharmacopoeia. [0003] Copper Aspirin [Cu(ASA) 2 ] 2 It is a new type of aspirin derivative, which has higher anti-inflammatory and anti-thrombotic effects than aspirin, and has less toxic and side effects. Research and development are carried out in the center, and the clinical research work has been basically completed. Matching its research and development, [Cu(ASA) 2 ] 2 The current purity analysis method and impurity determination method is high performance liquid chromatography internal standard method. When using this method...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/34G01N30/60G01N30/74
Inventor 刘祝东刘伟平普绍平高传柱何键
Owner KUNMING INST OF PRECIOUS METALS
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