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Method for separating and determining calcipotriol midbody L and related impurities

A technology for calcipotriol and intermediates, which is applied in the field of analytical chemistry, can solve the problems of not separating and measuring intermediates, etc., and achieves the effects of effective impurity control, high accuracy, and separation and measurement.

Active Publication Date: 2017-06-30
CHONGQING HUABANGSHENGKAI PHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is currently no HPLC method for the separation and determination of intermediate L and its related impurities

Method used

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  • Method for separating and determining calcipotriol midbody L and related impurities
  • Method for separating and determining calcipotriol midbody L and related impurities
  • Method for separating and determining calcipotriol midbody L and related impurities

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Example 1 related impurity M b , M b The 20S isomer, M c , M c Localization of the 20S isomer

[0049] (1) M b , M b The 20S isomer, M c , M c Preparation of the 20S isomer localization solution

[0050] m b Positioning solution: weigh the impurity M b 15.11mg, put it in a 50ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well, that is.

[0051] m c Positioning solution: weigh the impurity M c 15.26mg, put it in a 50ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well, that is.

[0052] m b 20S isomer localization solution: Weigh out the impurity M b 15.28 mg of the 20S isomer, put in a 50ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well, and you get it.

[0053] m c 20S isomer localization solution: Weigh out the impurity M c Put 15.22mg of 20S isomer in a 50ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well, and you get it.

[0054] (2) ...

Embodiment 2

[0056] Example 2 Calcipotriol intermediate L and related impurities M b , M b The 20S isomer, M c , M c Separation of the 20S isomer

[0057] (1) Intermediate L and related impurities M b , M b The 20S isomer, M c , M c Preparation of mixed solution of 20S isomers

[0058] Accurately pipette the M prepared in Example 1 respectively b , M c , M b The 20S isomer and the M c Put 3.3ml of each 20S isomer positioning solution in the same 100ml measuring bottle, add diluent to dilute to the mark, shake well to get a mixed positioning stock solution, then accurately weigh 10.26mg of intermediate L reference substance and put it in a 10ml measuring bottle , add 1.0ml of mixed positioning stock solution, then add diluent to dissolve and dilute to the mark, shake well to obtain a mixed solution.

[0059] (2) Take 20 μ l of the mixed solution for sample injection, carry out high-performance liquid chromatography analysis according to the above-mentioned chromatographic condit...

Embodiment 3

[0060] The separation and detection of embodiment 3 need testing product

[0061] (1) Preparation of the test solution: Take about 10 mg of the test product, put it in a 10 ml measuring bottle, add a diluent to dissolve it and dilute it to the mark, shake well, and you get it.

[0062] (2) Get need testing solution, mixed solution 20 μ l sample injections respectively, carry out high performance liquid chromatography analysis according to above-mentioned chromatographic condition, record chromatogram, the chromatogram of need testing solution is as follows Figure 7 As shown, no related impurity M was detected in the test solution. b , M b The 20S isomer, M c and M c The 20S isomer.

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Abstract

The invention belongs to the field of analytical chemistry and specifically relates to a method for separating and determining calcipotriol midbody L and related impurities. According to the method for separating and determining calcipotriol midbody L and related impurities, silica gel is taken as a solid phase and ethyl acetate-n-hexane is taken as a flowing phase for separating. According to the method, the calcipotriol midbody L and the related impurities can be effectively separated. The determining method comprises the following steps: by adopting a high performance liquid chromatography method, taking calcipotriol midbody L and related impurities reference substances and respectively preparing into a reference substance solution and a sample solution, performing high performance liquid chromatography analysis, recording chromatograms and comparing the impurity peak areas at corresponding peak time in the reference substance solution and the sample solution, thereby realizing the effective separation and detection of the calcipotriol midbody L and related impurities. The operation is simple and the accuracy is high.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for separating and measuring calcipotriol intermediate L and related impurities. Background technique [0002] The chemical name of calcipotriol is 9,10-cyclocholesta-24-cyclopropyl-5,7,10(19),22-tetraene-1,3,24 triol, and its molecular formula is C 27 h 40 o 3 , molecular weight: 412.61. Calcipotriol is mainly used in the topical treatment of psoriasis vulgaris. Compound L is an important intermediate for the synthesis of calcipotriol, and its structural formula is as follows: [0003] [0004] During the synthesis of intermediate L, various impurities such as M b , by-product M b The 20S-isomer, M c and M c The 20S-isomer etc., the structural formulas of these impurities are as follows: [0005] [0006] [0007] Among the above impurities, M b and its by-product M b The 20S-isomer contains some groups that are toxic, mutagenic or car...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/74G01N30/06
CPCG01N30/06G01N30/74
Inventor 周春燕曾正英
Owner CHONGQING HUABANGSHENGKAI PHARM
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