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A kind of related substance analysis method of calcium dibutyryl cyclophosphate or its preparation

A technology for calcium dibutyryl cyclophosphate adenosine phosphate and related substances, which is applied in the field of analytical chemistry, can solve the problems that cannot be separated and analyzed effectively at the same time, and the related substances are not controlled, and achieves the effects of strong specificity, high sensitivity and strong operability

Active Publication Date: 2015-12-30
SPH NO 1 BIOCHEM & PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome that the existing calcium dibutyrylcyclic adenosine monophosphate or its preparations do not control related substances, and the existing high performance liquid chromatography analysis conditions for content determination cannot effectively separate and analyze the two Butyryl cyclic adenosine monophosphate calcium or its preparations have defects in several main related substances, and a method for analyzing related substances of dibutyryl cyclic adenosine monophosphate calcium or its preparations is provided

Method used

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  • A kind of related substance analysis method of calcium dibutyryl cyclophosphate or its preparation
  • A kind of related substance analysis method of calcium dibutyryl cyclophosphate or its preparation
  • A kind of related substance analysis method of calcium dibutyryl cyclophosphate or its preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Analysis of Related Substances of Calcium Dibutyryl Cycloadenosine Phosphate

[0035] Adopt Alliancee2695 / 2489 high performance liquid chromatograph (Waters, the U.S.), ZorbaxSB-C 18 Chromatographic column (4.6*250mm, 5μm, Agilent), column temperature 25°C, injection volume 20uL, detection wavelength 273nm. In mobile phase, aqueous phase is phosphoric acid-potassium dihydrogen phosphate buffer solution (wherein, the concentration of potassium dihydrogen phosphate aqueous solution is 100mM, adds tetramethyl ammonium hydroxide (concentration is 1mM), pH value is 4.0), organic phase is Acetonitrile. The flow rate is 1.0mL / min, gradient elution is used, and the mobile phase ratio changes with time as shown in Table 2:

[0036] Table 2 mobile phase ratio

[0037] time (min)

Organic phase (%, v / v)

0

10

5

24

10

30

11

32

12

37

13

85

17

85

[0038] The analysis sample is calcium ...

Embodiment 2

[0041] Dibutyryl cyclic adenosine monophosphate calcium related substance analysis specificity test adopts Alliancee2695 / 2489 high performance liquid chromatograph (Waters, the U.S.), DiamonsilC 18 Column (4.6*250mm, 5μm, Dima Technology), column temperature 40°C, injection volume 10μL, detection wavelength 273nm. The aqueous phase of the mobile phase is a formic acid-sodium formate buffer solution (wherein the concentration of the sodium formate aqueous solution is 50 mM, and the pH value is 3.0), and the organic phase is acetonitrile. The flow rate was 1.0 mL / min, gradient elution was adopted, and the gradient change was the same as in Example 1, except that the initial proportion of the organic phase was 5%, and the final proportion was 90%.

[0042] The sample is calcium adenosine dibutyryl cycloadenosine monophosphate bulk drug (manufactured by Shanghai First Biochemical Pharmaceutical Co., Ltd. Institute of Materia Medica, batch number 101108), prepared into a 1.0 mg / mL ...

Embodiment 3

[0054] Determination of Related Substances of Calcium Dibutyryl Cycloadenosine Phosphate

[0055] Adopt Alliancee2695 / 2489 high performance liquid chromatograph (Waters, U.S.), DiamonsilC 18 Column (4.6*250mm, 5μm, Dima Technology), column temperature 25°C, injection volume 20μL, detection wavelength 273nm. The aqueous phase of the mobile phase is an inorganic salt buffer solution with a pH value of 3.0 (phosphoric acid-potassium dihydrogen phosphate buffer, formic acid-ammonium formate buffer, acetic acid-sodium acetate buffer, the specific buffer salt type is shown in Table 4), The organic phase is acetonitrile, and the flow rate is 0.8mL / min. Gradient elution is adopted. The gradient change is the same as in Example 1. The difference is that the types and concentrations of inorganic salts in the inorganic salt buffer solution are different. The inorganic salts are selected from potassium dihydrogen phosphate, ammonium formate and Sodium acetate.

[0056] The sample is thr...

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Abstract

The invention discloses a related substance analysis method for calcium dibutyryladenosine cyclophosphate or a preparation thereof. The related substance analysis method comprises the step of analyzing the calcium dibutyryladenosine cyclophosphate or the preparation thereof by using a high performance liquid chromatography. A mobile phase in the high performance liquid chromatography is an inorganic salt buffering solution and a polarity organic solvent with the pH (Potential of Hydrogen) value of 1.0-6.0. The related substance analysis method for the calcium dibutyryladenosine cyclophosphate or the preparation thereof disclosed by the invention can be used for conveniently and rapidly controlling a plurality of main related substances of the calcium dibutyryladenosine cyclophosphate or the preparation thereof; the precision and the flexibility are high; the invention provides an effective method for formulating and improving quality standards of the related substances of bulk pharmaceutical chemicals of the drug or the preparation thereof.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and relates to an analysis and detection method of chemical medicine or its preparation, in particular to an analysis method of related substances of dibutyryl cyclic adenosine monophosphate calcium or its preparation. Background technique [0002] Intracellular cyclic adenosine monophosphate (cAMP) can transmit hormone information to enable cells to produce corresponding functions. For example, the positive inotropic effect of catecholamines is caused by the increase of intracellular cAMP. However, exogenous cAMP cannot penetrate the cell membrane and thus cannot produce positive inotropic effects. Butyrylated cyclic adenosine monophosphate such as 2′-O-dibutyryl cyclic adenosine monophosphate or N 6 -Monobutyryl cyclic adenosine monophosphate is a derivative of cAMP, which can penetrate the cell membrane and has a destructive effect on phosphodiesterase in vivo. Therefore, in vivo experimen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 黄臻辉琚姝霍建丽贾存宇
Owner SPH NO 1 BIOCHEM & PHARMA CO LTD
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