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Method for detecting drug and enantiomer impurities of drug

A technology for enantiomers and impurities, which is applied in the field of simultaneous detection of drugs and their enantiomer impurities, can solve problems such as no reports of high-performance liquid chromatography analysis methods, and achieves short running time, loose requirements, and detection. Finished low effect

Active Publication Date: 2014-09-24
HEFEI COSOURCE PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] There is no report on the high performance liquid chromatography analysis method of the compound of formula (I) and formula (II) in the literature

Method used

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  • Method for detecting drug and enantiomer impurities of drug
  • Method for detecting drug and enantiomer impurities of drug
  • Method for detecting drug and enantiomer impurities of drug

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (a) Pre-column derivation:

[0030] Dissolve 10mg of S-Xemilofiban hydrochloride in 8ml of dichloromethane, react with 0.5ml of triethylamine and 15mg of p-nitrobenzoyl chloride at room temperature for 60min, add 0.2ml of diethylamine, place it for 20min, and place it in a water bath at 60°C The solvent was evaporated to dryness, and the residue was dissolved in absolute ethanol and adjusted to 20ml (concentration of about 0.5mg / ml) as the raw material for the test solution. Take an appropriate amount of R-Xemilofiban hydrochloride reference substance according to the law to prepare a solution with a concentration of about 10 μg / ml as the enantiomer positioning solution. In addition, S-Xemilofiban hydrochloride reference substance and R-Xemilofiban hydrochloride reference substance were prepared according to the law to prepare solutions with concentrations of 0.5mg / ml and 2.5μg / ml respectively as system suitability solutions.

[0031] b) HPLC analysis and UV detection:...

Embodiment 2

[0036] Embodiment 1 methodological verification result

[0037] 1. Limit of detection and limit of quantitation

[0038] A signal-to-noise ratio of 3:1 was used as the detection limit, and a signal-to-noise ratio of 10:1 was used as the lowest quantification limit.

[0039] Component

The lowest concentration limit of quantification (μg / ml)

Minimum detection limit concentration (μg / ml)

S-Xemilofiban derivatives

0.0503

0.0201

R-Xemilofiban derivatives

0.0513

0.0205

[0040] 2. Linearity and range

[0041] According to embodiment 1 chromatographic conditions, inject liquid chromatograph respectively, record chromatogram, carry out linear regression to peak area (Y) by solution concentration (X), get regression equation

[0042]

[0043]

[0044] 3. Accuracy

[0045] Weigh about 10.0 mg of 9 parts of S-Xemilofiban, prepare the test solution according to the derivatization method, and add 0.25%, 0.5%, and 0.75% of the ...

Embodiment 3

[0061] Isolation of S-Xemilofiban hydrochloride composition

[0062] (a) Pre-column derivation:

[0063] Dissolve 10 mg of S-Xemilofiban hydrochloride for injection (containing excipients such as mannitol) (calculated as S-Xemilofiban hydrochloride) in 10 ml of absolute ethanol, centrifuge, and evaporate the supernatant to dryness. Dissolve the residue in 8ml of dichloromethane, add 0.5ml of triethylamine and 15mg of p-nitrobenzoyl chloride, react at room temperature for 60min, add 0.2ml of diethylamine, let stand for 20min, evaporate the solvent to dryness in a water bath at 60°C, and use Dissolve in absolute ethanol and set the volume to 20ml preparation need testing solution. Another prescription amount of blank excipients was prepared according to law as a blank excipient solution.

[0064] b) HPLC analysis and UV detection:

[0065] With embodiment 1.

[0066] see attached results Figure 4 with 5 .

[0067] Figure 4 with Figure 5 Display: the blank excipient s...

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Abstract

The invention relates to the technical field of chemical analysis, in particular to a method for detecting a drug and enantiomer impurities of the drug. The method is characterized in that a sample to be detected, organic amine and acyl chloride are subjected to derivatization reaction, a reaction resultant is separated through a chirality chromatographic column by the adoption of high performance liquid chromatography and detected through an ultraviolet detector, and then the content is obtained through calculation. The method is stable, practicable and easy, convenient and rapid to implement.

Description

technical field [0001] The invention relates to the technical field of chemical analysis, in particular to a method for simultaneously detecting impurities of medicines and their enantiomers. Background technique [0002] The compound of formula (I), English name S-Xemilofiban, is a reversible antagonist of non-peptide platelet glycoprotein (GP) IIb / IIIa receptor, which is the main platelet surface receptor related to the platelet aggregation process. body. S-Xemilofiban prevents the binding of fibrinogen to glycoprotein IIb / IIIa, thereby blocking the cross-linking of platelets and the aggregation of platelets. [0003] S-Xemilofiban has a chiral center, and the structural formula of its enantiomer R-Xemilofiban is formula (II). During the process of synthesizing S-Xemilofiban, there may be a by-product R-Xemilofiban, namely its enantiomer impurity. The control of enantiomeric impurity limits is an important part of the quality control of compounds, especially drugs, and i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 高署王晓玲程开生孙宏张石刘玉
Owner HEFEI COSOURCE PHARMA CO LTD
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