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Method for separation and determination of optical isomer impurities of bepotastine besilate

A technology of bepotastine bepotastine and optical isomers, which is applied in the field of separation and determination of optical isomer impurities of drugs, can solve the problems of decreased column efficiency, broadened peak shape, and poor durability of chromatographic columns, achieving flow Simple preparation, high column efficiency and good durability

Active Publication Date: 2018-02-23
CHONGQING HUAPONT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The ULTRON ES-CD column has an unsatisfactory separation effect on the two optical isomers of bepotastine besilate, and after about one month of use, the two isomers can hardly be separated;
[0008] ULTRON ES-OVM column packing is oval protein-bonded silica gel, which can effectively separate bepotastine and its isomers, but after a period of use, the peak shape becomes wider, the column efficiency decreases significantly, and the durability of the chromatographic column is poor

Method used

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  • Method for separation and determination of optical isomer impurities of bepotastine besilate
  • Method for separation and determination of optical isomer impurities of bepotastine besilate
  • Method for separation and determination of optical isomer impurities of bepotastine besilate

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Experimental program
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Embodiment 1

[0039] Example 1 Chiralpak AD-H chromatographic column normal phase HPLC (high performance liquid chromatography) detection

[0040] Chromatographic conditions

[0041] Chromatographic column: Chiralpak AD-H (filler is silica gel coated with amylose-tris(3,5-xylylcarbamate), 4.6×250mm, 5μm)

[0042] Mobile phase: n-hexane-ethanol-ethanolamine (87:13:0.1, V / V / V); n-hexane and ethanol used are chromatographically pure, and ethanolamine is analytically pure

[0043] Detection wavelength: 260nm;

[0044] Injection volume: 20μl; The number of theoretical plates is not less than 2000 based on the peak of bepotastine besilate

[0045] Method: Take appropriate amount of bepotastine bepotastine reference substance and R-isomer reference substance respectively, add appropriate amount of ethanol and ultrasonically dissolve them, and dilute to the mark with n-hexane to make about 1 mg of bepotastine besilate and R-isomer reference substance per 1 ml. For the mixed solution of 50 μg o...

Embodiment 2

[0061] Determination of Optical Isomer Content in Bepotastine Bepotastine Tablets in Embodiment 2

[0062] Carry out normal phase HPLC determination by aforementioned method, instrument and chromatographic condition, concrete operation is as follows:

[0063] Take an appropriate amount of bepotastine bepotastine reference substance and R-isomer reference substance respectively, add appropriate amount of ethanol and ultrasonically dissolve them, and dilute to the mark with n-hexane to make about 1 mg of bepotastine besilate and R-isomer According to the above chromatographic conditions, inject 20 μl of the mixed solution with 5 μg of the body, and record the chromatogram. The sequence of peaks is bepotastine and R-isomer in turn, the number of theoretical plates calculated based on the peak of bepotastine should not be less than 2000, and the degree of separation between bepotastine and adjacent isomers should not be less than 2.0.

[0064] Take three consecutive batches of be...

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Abstract

A method for splitting a Bepotastine Besilate optical isomer and quantitatively measuring R-isomer impurity is disclosed. According to the invention, high performance liquid chromatography is adopted. A mobile phase contains n-hexane and ethanol. The method is characterized in that normal-phase liquid chromatography is adopted; packing used in a chromatographic column is silica gel with its surface coated with amylase-tris-(3,5-xylyl carbamate); and the mobile phase also contains an alkaline additive. In comparison with the prior art, the method provided by the invention has advantages as follows: the mobile phase is simple to prepare, and resolutions of two isomers are both within 4.5-5.5. Especially, the chromatographic column of the method has good durability, and the chromatographic column still has high column efficiency after having been used for one year. Thus, analytic determination cost is greatly reduced.

Description

Technical field: [0001] The invention relates to a method for separating and measuring optical isomer impurities of medicines, in particular to separating bepotastine besilbestatin and its R-isomer by high performance liquid chromatography and quantitatively determining the content of the R-isomer method. Background technique: [0002] Bepotastine bepotastine is a non-sedating highly selective histamine H1 receptor antagonist drug with anti-allergic and antipruritic effects. [0003] Bepotastine bepotastine is a chiral compound with S-configuration, chemical name (+)-(S)-4-[4-[(4-chlorophenyl)(2-pyridine)methoxy]piperidine ] Butyric acid benzene sulfonate, and its R-isomer has a big difference in pharmacological action, and bepotastine besilate is superior to the R-isomer. [0004] In the pharmaceutical process, the R-isomer of bepotastine besilate is often monitored as an impurity. Therefore, the separation of bepotastine bepotastine (S-configuration) and the R-isomer an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 赵静许佳肖丽黄真
Owner CHONGQING HUAPONT PHARMA
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