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Method for detecting impurity in bexarotene softgel by high performance liquid chromatography

A high-performance liquid chromatography and soft capsule technology, which is applied in the field of high-performance liquid chromatography for detecting impurities in besarotene soft capsules, can solve problems such as undocumented impurity detection methods and the like

Active Publication Date: 2019-11-15
HUMANWELL PURACAP PHARM WUHAN CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] During the research process, it was found that there are 3 kinds of impurities that can be identified in Besarotene Soft Capsules, which are impurity a: Impurity b: As well as keto acid impurities, the structural formulas of bexarotene and its impurity a and impurity b are very similar, and the polarity of the functional groups is similar, so it is very important to use a certain method to effectively separate them, and the United States Pharmacopoeia (abbreviated as USP ) has not yet recorded the detection method of impurities in Besarotene soft capsules

Method used

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  • Method for detecting impurity in bexarotene softgel by high performance liquid chromatography
  • Method for detecting impurity in bexarotene softgel by high performance liquid chromatography
  • Method for detecting impurity in bexarotene softgel by high performance liquid chromatography

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preparation example Construction

[0037] The preparation method of mobile phase A is: thoroughly mix 700mL acetonitrile and 300mL 0.01M ammonium acetate buffer and degas; the preparation method of mobile phase B is: thoroughly mix 800mL acetonitrile and 200mL 0.01M ammonium acetate buffer gas; the preparation method of 0.01M ammonium acetate buffer solution is: dissolve 0.77g ammonium acetate in 1L deionized water, and adjust the pH of the solution to 3.0 with glacial acetic acid.

[0038] Tests have proved that the contents of bexarotene soft capsules are insoluble in water, but soluble in more polar organic solvents, such as methanol and acetonitrile, and the capsule shell is insoluble in methanol at room temperature. Therefore, methanol was chosen as the diluent.

[0039] Preparation of reference substance stock solution: Weigh 6.0 mg of bexarotene standard substance into a 100mL volumetric flask, add diluent to dilute to the mark, and shake well to obtain a reference substance stock solution with a bexarot...

Embodiment 1

[0045] Good system adaptability:

[0046] It has been verified that the diluent does not interfere with the main peak, the theoretical plate number of the main peak is 18501, the tailing factor of the main peak is 1.1, and the RSD of the first 6 sequences against the main peak area of ​​the standard solution is 0.2%.

Embodiment 2

[0048] Resolution: (1) The diluent and blank excipients do not interfere with the main peak of besarotene, related substance a, related substance b, and keto acid impurity peak; (2) The resolution between the main peak and adjacent peaks is 11.5; (3) The retention times and relative retention times of the main peak and each impurity peak are shown in Table 1.

[0049] Table 1 Retention time and relative retention time of main peak and each impurity peak

[0050] name betha rotten Impurity a Impurity b Keto acid impurities Types of raw material process impurities process impurities process impurities keep time 16.82 24.25 41.05 8.30 relative retention time -- 1.4 2.4 0.5

[0051] Strong degradation test: (1) The impurity peaks produced in any strong degradation test do not interfere with the main peak, (2) The peak purity threshold of the main peak is greater than the peak purity angle of the reference substance and the degra...

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Abstract

The invention provides a method for detecting impurity in bexarotene softgel by high performance liquid chromatography. In the high performance liquid chromatography, mobile phases A and B are included; the mobile phase A includes acetonitrile and a 0.01M ammoniom acetate buffer in the proportion of 70 to 30; the mobile phase B includes acetonitrile and a 0.01M ammoniom acetate buffer in the proportion of 80 to 20; and the pH value of the ammoniom acetate buffer is 3.0. Via the detection method, the impurity in the bexarotene softgel can be detected simply and rapidly, different peaks can be separated effectively, and the detection method is also simple in operation and shorter in analysis time.

Description

technical field [0001] The invention relates to the field of medicine, in particular to a method for detecting impurities in bexarotene soft capsules by using high performance liquid chromatography. Background technique [0002] Bexarotene soft capsule is a retinoic acid monokinase inhibitor, which selectively binds and activates retinoic acid receptors to control cell differentiation and proliferation. It is administered orally to treat skin symptoms of refractory cutaneous T-cell lymphoma. Developed by American Ligand Pharmaceutical Company, the main component of the soft capsule is 4-[1-(5,6,7,8-tetrahydro-3,5,5,8,8-pentamethyl-2-naphthyl) vinyl] Benzoic acid, in addition polysorbate, povidone K 90, macrogol 400, tert-butylhydroxyanisole (BHA). Capsule shell ingredients include gelatin, glycerin, purified water. [0003] During the research process, it was found that there are 3 kinds of impurities that can be identified in Besarotene soft capsules, which are impurity a...

Claims

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/8872
Inventor 孔雪阳刘波叶翔蔡波涛邹玲玲徐欣
Owner HUMANWELL PURACAP PHARM WUHAN CO LTD
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