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Analysis method for detecting impurity in aspartate ornithine

A technique for aspartic acid ornithine and analytical methods, applied in the field of analytical chemistry, can solve the problem that there is no clear collection of quantitative and qualitative methods, and there is no disclosure of dimeric arginine and α-aspartic acid dimer gates Problems such as qualitative and quantitative analysis methods of aspartic acid condensates to achieve good resolution

Active Publication Date: 2018-07-06
SHANDONG INST FOR FOOD & DRUG CONTROL
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0004] Regarding the detection method of impurities in aspartic acid ornithine, CN104807924A aspartic acid ornithine raw material and preparation specific impurity detection method provides a method for accurately analyzing and detecting the aspartic acid ornithine prepared by the synthesis process. Contained impurities: a high-efficiency liquid phase analysis and detection method for fumaric acid, arginine, urea, succinic acid, malic acid, and lactam; CN102288687A An analysis and detection method for aspartic acid ornithine impurities also only provides Ornithine or impurity ornithine-containing drugs and preparations of ornithine detection method; the above patents do not disclose dimer arginine, α-aspartic acid dimer, aspartic acid condensation Qualitative and quantitative analysis methods of substances
Moreover, the quantitative and qualitative methods for the above four impurities are not clearly included in the existing drug quality standards for aspartic acid ornithine and its preparations. This application is mainly aimed at the qualitative and quantitative methods of the above four impurities. Research

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  • Analysis method for detecting impurity in aspartate ornithine
  • Analysis method for detecting impurity in aspartate ornithine
  • Analysis method for detecting impurity in aspartate ornithine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Example 1 Resolution detection

[0049] 1). Specific experimental operations:

[0050] Positioning solution of each impurity reference substance: accurately weigh out 10 mg of 3-amino-2-piperidone, α-aspartic acid dimer, aspartic acid condensate, and dimer arginine, and put them into 50 ml measuring bottles. In the medium, add mobile phase B to dissolve and dilute to the mark, shake well, and get ready.

[0051] Positioning solution for the test product: accurately weigh 100 mg of ornithine hydrochloride, aspartic acid, and ornithine aspartate, respectively, put them in a 10 ml measuring flask, add mobile phase B to dissolve and dilute to the mark, shake well, that is Got.

[0052] Mixed solution: accurately weigh ornithine aspartate, place it in a 10ml measuring flask, accurately measure 3-amino-2-piperidone, α-aspartic acid dimer, aspartic acid condensate, Place 0.5ml of the dimer arginine reference substance positioning solution in the same place, add mobile phase B to dis...

Embodiment 2

[0058] Example 2 Measurement of linear range

[0059] 1) Solution configuration

[0060] Precisely weigh 10mg each of α-aspartic acid dimer, aspartic acid condensate, and dimer arginine, put them in a 10ml volumetric flask, add an appropriate amount of solvent to dissolve and dilute to the mark, shake well, as impurities Linear stock solution.

[0061] Precisely weigh each 10mg of aspartic acid and ornithine, and place them in a 10ml measuring flask. Precisely add 2ml of the above-mentioned impurity linear stock solution and place in a 100ml measuring flask. Add an appropriate amount of solvent to dissolve and dilute to the mark. Shake well, as linear Test solution 1#.

[0062] Precisely measure linear test solution 1#8ml, 7ml, 6ml, 5ml, 4ml, 3ml, 2.5ml, 1ml, 0.5ml, put them into 10ml measuring flasks, add solvent to dilute to the mark, shake well, and use as linear test solution 2# , 3#, 4#, 5#, 6#, 7#, 8#, 9#, 10#.

[0063] Accurately weigh 40mg of 3-amino-2-piperidone into a 100ml...

Embodiment 3

[0088] Example 3 Determination of detection limit

[0089] 1), the method of detection limit determination

[0090] Configuration of detection limit solution: Dilute the linear stock solution of each impurity in Example 2 step by step, and obtain the solution when S / N≈3 as the detection limit solution;

[0091] 2), measurement results

[0092] Precisely take 20μl of the blank solution and inject it into the liquid chromatograph; Precisely take 20μl of the above-mentioned limit of quantification solution, inject it into the liquid chromatograph, and inject 3 consecutive samples, record the chromatogram, take S / N≈3 as the detection limit, and the statistics are as follows .

[0093] Table 8: Detection limit test results

[0094]

[0095] Test results: The detection limit of aspartic acid condensate was 0.6ng, the detection limit of α-aspartic acid dimer was 1.0ng, the detection limit of dimer arginine was 3.4ng, and the detection limit of ornithine was 16.7ng. The detection limit of aspa...

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Abstract

The invention discloses an analysis method for detecting impurities in aspartate ornithine and belongs to the field of analytical chemistry. The analysis method comprises the following steps: by usingliquid chromatography, under the conditions that an amino bonded silica gel filling agent, namely Thermo APS-2 of 4.6 mm*250 mm*5 [mu]m, is adopted, 0.1 mol / L monopotassium phosphate buffer solution-acetonitrile (35:65) is used as a mobile phase A, 0.1 mol / L monopotassium phosphate buffer solution-acetonitrile (50: 50) is used as a mobile phase B, a detection wavelength is 200 nm, a flowing speedis 1.0 ml / minute, and a column temperature is 30 DEG C, performing gradient elution, and performing analysis. By adopting the technical scheme, impurities such as 3-amino-2-piperidone, di-poly-l-arginine and an alpha-aspartate biopolymer and an aspartate condensation compound can be rapidly and accurately qualitatively and quantitatively analyzed, a good separation degree can be achieved, a relatively low detection limit and quantitative limit can be achieved, a relatively wide linear range can be achieved, the contents of different impurities can be relatively accurately calculated, and technical support can be provided for further monitoring and studying impurities in the aspartate ornithine.

Description

[0001] Technical Field: The present invention belongs to the field of analytical chemistry, and specifically relates to a method for the analysis and detection of ornithine aspartate impurities using HPLC method, and more specifically, to a method for the analysis and detection of ornithine aspartate in 3- Amino-2-piperidone, dimer arginine, α-aspartic acid dimer, aspartic acid condensate four impurities method. Background technique: [0002] Ornithine aspartate (chemical name (S)-2,5-diaminovaleric acid (s)-2-aminosuccinate), used in clinical practice in Germany in the 1970s, and collected in 1991 The German Pharmacopoeia was imported and marketed in China in 2000. It was produced and marketed by domestic manufacturers in 2006. It is used to treat hyperammonemia caused by liver disease. Ornithine aspartate can provide a substrate for the synthesis of urea and glutamine in the body. Under physiological and pathological conditions, the synthesis of urea and glutamine will be affec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 张冬梅牛冲于明艳赵海云李玉杰冷佳蔚
Owner SHANDONG INST FOR FOOD & DRUG CONTROL
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