Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of assay method of trifluoroacetic acid in bivalirudin

A kind of technology of trifluoroacetic acid and determination method, applied in the field of medicine, can solve problems such as difficult chromatographic column elution

Active Publication Date: 2015-09-02
WUHAN WUYAO SCI & TECH
View PDF0 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to solve the above problems, the technical scheme of the present invention provides a detection method, which overcomes the shortcoming that bivalirudin is not easy to elute from the chromatographic column

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of assay method of trifluoroacetic acid in bivalirudin
  • A kind of assay method of trifluoroacetic acid in bivalirudin
  • A kind of assay method of trifluoroacetic acid in bivalirudin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Embodiment 1: one of the content determination of trifluoroacetic acid in bivalirudin:

[0040] 1. Experimental equipment and chromatographic conditions

[0041] Dianne U3000 high performance liquid chromatography, Ilite C18 column (5μm, 4.6*200mm), using 0.05% phosphoric acid solution (adjust the pH value to 3.01 with 10% sodium hydroxide solution) as mobile phase A, and methanol as mobile phase B , carry out gradient elution; the flow rate is 0.8-1.5ml / min; the column temperature is 25-35°C; the detection wavelength is 200-220nm, and the gradient elution procedure is as follows:

[0042]

[0043] 2. Determination of samples

[0044]Accurately weigh an appropriate amount of trifluoroacetic acid reference substance, use mobile phase (mobile phase A is 0.05% phosphoric acid solution, phosphoric acid solution should use 10% sodium hydroxide solution to adjust the pH value to 3.01, mobile phase B is methanol, mobile phase A:B 95:5V / V) to prepare a solution containing ...

Embodiment 2

[0045] Embodiment 2: the content determination two of trifluoroacetic acid in bivalirudin:

[0046] 1. Experimental equipment and chromatographic conditions

[0047] Dianne U3000 high performance liquid chromatography, Ilite C18 column (5μm, 4.6*200mm), with 0.08% phosphoric acid solution (adjust the pH value to 4.00 with 10% sodium hydroxide solution) as mobile phase A, and methanol as mobile phase B , carry out gradient elution; the flow rate is 0.8-1.5ml / min; the column temperature is 25-35°C; the detection wavelength is 200-220nm, the gradient elution method, including the concentration of the mobile phase, and the elution time are as follows:

[0048]

[0049] 2. Determination of samples

[0050] Precisely weigh an appropriate amount of trifluoroacetic acid reference substance, use mobile phase (mobile phase A is 0.08% phosphoric acid solution, phosphoric acid solution should be adjusted to pH 4.00 with 10% sodium hydroxide solution, mobile phase B is methanol, mobile...

Embodiment 3

[0051] Embodiment 3: three of content determination of trifluoroacetic acid in bivalirudin:

[0052] 1. Experimental equipment and chromatographic conditions

[0053] Dianne U3000 high performance liquid chromatography, Ilite C18 column (5μm, 4.6*200mm), with 0.10% phosphoric acid solution (adjust the pH value to 3.51 with 10% sodium hydroxide solution) as mobile phase A, and methanol as mobile phase B , carry out gradient elution; the flow rate is 0.8-1.5ml / min; the column temperature is 25-35°C; the detection wavelength is 200-220nm, and the gradient elution procedure is as follows:

[0054]

[0055] 2. Determination of samples

[0056] Accurately weigh an appropriate amount of trifluoroacetic acid reference substance, use mobile phase (mobile phase A is 0.10% phosphoric acid solution, phosphoric acid solution should use 10% sodium hydroxide solution to adjust the pH value to 3.51, mobile phase B is methanol, mobile phase A:B 98:2V / V) to prepare a solution containing 1m...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention belongs to the technical field of medicines and particularly relates to a method for determining the content of trifluoroacetic acid in bivalirudin. The detection method is a high performance liquid chromatography. The invention provides one detection method which overcomes the disadvantage that the bivalirudin is not easy to elute from a chromatographic column. The technical scheme provided by the invention has the characteristics that a phosphoric acid solution is used as a mobile phase A and methanol is used as a mobile phase B, wherein the mobile phase A is a 0.05%-0.10% phosphoric acid solution; the pH (Potential of Hydrogen) value of the phosphoric acid solution is adjusted to 3.01-4.00 by using a 10% sodium hydroxide solution. With the adoption of a gradient eluting manner, the gradient eluting manner can be used for very easily eluting the bivalirudin from the chromatographic column.

Description

Technical field: [0001] The invention belongs to the technical field of medicine, and in particular relates to a method for determining the content of trifluoroacetic acid in bivalirudin by high performance liquid chromatography. Background technique: [0002] Bivalirudin is a new type of anticoagulant. The anticoagulant component is a hirudin derivative (fragment), which is a synthetic 20-peptide with a relative molecular weight of 2180. This product is a direct, specific and reversible inhibitor of thrombin. Whether thrombin is in the blood circulation or combined with thrombus, this product can specifically bind to its catalytic site and anion binding site (also known as substrate recognition site), thereby directly inhibiting the activity of thrombin. Because thrombin can hydrolyze the peptide bond between Arg3 and Pro4 in the peptide sequence of this product, this product is inactivated, so the inhibitory effect of this product on thrombin is reversible and short-lived...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/36G01N30/02
Inventor 吴雪英乔春莲于艳春杨波耿海明
Owner WUHAN WUYAO SCI & TECH