Ziconotide and impurity detection method

A technology of ziconotide and impurities, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of large polarity difference, difficulty in effective separation, waste of manpower and material resources, etc.

Inactive Publication Date: 2014-06-25
HYBIO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0019] Judging from the structures of the above compounds, their structures are very similar, and from the perspective of polarity, there are some impurities that have a large polarity difference with ziconotide. It is very difficult to separate effectively
[0020] U...

Method used

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  • Ziconotide and impurity detection method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] 1. Instrument conditions

[0055] High performance liquid chromatography: Waters2695

[0056] Chromatographic column: Kromasil C18 (250mm×4.6mm);

[0057] Flow rate: 1.0ml / min

[0058] Column temperature: 40°C

[0059] Injection volume: 20μl

[0060] Mobile phase: mobile phase A is 0.01M potassium dihydrogen phosphate aqueous solution: acetonitrile = 90:10 (after the buffer solution and acetonitrile are fully mixed, adjust the pH to 6.5 with triethylamine), mobile phase B is 0.01M potassium dihydrogen phosphate aqueous solution: Acetonitrile (after the buffer solution and acetonitrile are fully mixed, adjust the pH to 6.5 with triethylamine) = 50:50, the gradient of the mobile phase is shown in Table 3 below.

[0061]

[0062] Get ziconotide and its intermediates and impurities, and use the mobile phase at 0 minutes to dissolve and prepare a test sample solution with a concentration of 1 mg / mL. Set the flow rate to 1.0ml / min, the detection wavelength to 230nm, a...

Embodiment 2

[0067] 1. Instrument conditions

[0068] High performance liquid chromatography: Waters2695

[0069] Chromatographic column: Kromasil C18 (150mm×4.6mm);

[0070] Flow rate: 1.0ml / min

[0071] Column temperature: 0°C

[0072] Injection volume: 20μl

[0073] Mobile phase: mobile phase A is 0.01M potassium dihydrogen phosphate aqueous solution (triethylamine adjusts pH=6.5), mobile phase B is 0.01M potassium dihydrogen phosphate aqueous solution: acetonitrile=40:60 (after the buffer and acetonitrile are fully mixed, Adjust pH=6.5 with triethylamine), see Table 5 below.

[0074]

[0075] Take ziconotide and its impurities, and use appropriate medium to dilute and dissolve to prepare the test sample solution. Set the flow rate to 1.0ml / min, the detection wavelength to 230nm, and the column temperature to 40°C. Take 20 μl of the test sample solution and inject it into the liquid chromatograph. The measurement results are shown in Table 6.

[0076]

[0077]

[0078] Un...

Embodiment 3

[0080] Instrument conditions

[0081] High performance liquid chromatography: Waters2695

[0082] Chromatographic column: Kromasil C18 (150mm×4.6mm);

[0083] Flow rate: 1.0ml / min

[0084] Column temperature: 40°C

[0085] Injection volume: 20μl

[0086] Mobile phase: mobile phase A is 0.01M sodium dihydrogen phosphate aqueous solution: acetonitrile=85:15 (after the buffer and acetonitrile are fully mixed, adjust the pH to 6.5 with triethylamine), mobile phase B is 0.01M sodium dihydrogen phosphate aqueous solution: Acetonitrile=50:50 (after the buffer solution and acetonitrile are fully mixed, adjust the pH to 6.5 with triethylamine), see Table 7 below.

[0087]

[0088] Take ziconotide and its impurities, and use appropriate medium to dilute and dissolve to prepare the test sample solution. Set the flow rate to 1.0ml / min, the detection wavelength to 230nm, and the column temperature to 40°C. Take 20 μl of the test sample solution and inject it into the liquid chromat...

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Abstract

The invention relates to a high performance liquid chromatography (HPLC) method for effective separating and analysis of ziconotide and impurities thereof.

Description

technical field [0001] The present invention relates to a high performance liquid chromatography (HPLC) method for effectively separating and analyzing ziconotide and its impurities. Background technique [0002] Ziconotide (Ziconotide) is a calcium ion channel inhibitor with analgesic effect. Ziconotide can produce significant analgesic effects in patients with severe chronic pain who are ineffective on opioid and non-steroidal analgesics, and it will not cause addiction and drug resistance. [0003] Patent CN101709082 mentions a preparation process of solid-phase synthesis of ziconotide. In the chemical synthesis process of ziconotide, there are several key intermediate steps, so the corresponding intermediates may remain in the final product. Therefore, it is very necessary to establish a separation and analysis method for the quality control of its intermediates and impurities. [0004] The structures of Ziconotide and its impurities are as follows: [0005] 1) Zicono...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 康旭宓鹏程马亚平袁建成
Owner HYBIO PHARMA
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