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Method for separating and determining calcipotriene starting raw material A and related impurities

A calcipotriol and raw material technology, applied in the field of analytical chemistry, can solve the problems of inaccurate quantification and low sensitivity of ultraviolet detectors, and achieve the effects of effective separation, high sensitivity and strong specificity

Active Publication Date: 2018-01-30
CHONGQING HUABANGSHENGKAI PHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Because calcipotriol starting material A and its impurity A 1 、A 2 、A 3 、A 4 and A 5 It has the characteristics of weak or no ultraviolet absorption, so the sensitivity of conventional ultraviolet detectors is not high and cannot be accurately quantified. At present, there is no HPLC method for the separation and determination of calcipotriol starting material A and its impurities

Method used

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  • Method for separating and determining calcipotriene starting raw material A and related impurities
  • Method for separating and determining calcipotriene starting raw material A and related impurities
  • Method for separating and determining calcipotriene starting raw material A and related impurities

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] 1. Instruments and conditions

[0073] Instrument: high performance liquid chromatography;

[0074] Chromatographic column: Agilent ZORBAX SIL (4.6×250mm, 5μm);

[0075] Mobile phase: n-hexane:isopropanol=90:10(V:V);

[0076] UV detector detection wavelength: 200nm;

[0077] Column temperature: 30°C;

[0078] Flow rate: 1.0ml / min;

[0079] Injection volume: 10μl;

[0080] Diluent: The mobile phase is n-hexane:isopropanol=90:10 (V:V).

[0081] 2. Experimental steps

[0082] (1)A 1 Reference substance solution stock solution: Accurately weigh A 1 100.01mg plus diluent dissolved to make 5.05mg / mL A 1 Reference substance solution stock solution;

[0083] (2)A 2 Reference substance solution stock solution: Accurately weigh A 2 102.55mg plus diluent dissolved to make 5.12mg / mL A 2 Reference substance solution stock solution;

[0084] (3)A 3 Reference substance solution stock solution: Accurately weigh A 3 101.27mg plus diluent dissolved to make 5.06mg / mL A ...

Embodiment 2

[0092] 1. Instruments and conditions

[0093] Instrument: high performance liquid chromatography;

[0094] Chromatographic column: Agilent ZORBAX SIL (4.6×250mm, 5μm);

[0095] Mobile phase: n-hexane:isopropanol=95:5(V:V);

[0096] Evaporative photodetector conditions: drift tube temperature: 51.0°C;

[0097] Gas flow rate: 1.7L / min;

[0098] Air pressure: 0.5Mpa;

[0099] Column temperature: 30°C;

[0100] Flow rate: 1.0ml / min;

[0101] Injection volume: 10μl;

[0102] Diluent: The mobile phase is n-hexane:isopropanol=95:5 (V:V).

[0103] 2. Experimental steps

[0104] (1)A 1 Reference substance solution stock solution: Accurately weigh A 1 100.01mg plus diluent dissolved to make 5.05mg / mL A 1 Reference substance solution stock solution;

[0105] (2)A 1 Positioning solution: precise measurement of A 1 Put 1.0ml of the reference substance solution stock solution in a 10ml measuring bottle, add diluent to dilute to constant volume, shake well, and obtain;

[0106]...

Embodiment 3

[0120] 1. Instruments and conditions

[0121] Instrument: high performance liquid chromatography;

[0122] Chromatographic column: Agilent ZORBAX SIL (4.6×250mm, 5μm);

[0123] Mobile phase: n-hexane:isopropanol=99.5:0.5(V:V);

[0124] Evaporative photodetector conditions: drift tube temperature: 42°C;

[0125] Gas flow rate: 1.7L / min;

[0126] Air pressure: 0.5Mpa;

[0127] Column temperature: 30°C;

[0128] Flow rate: 1.0ml / min;

[0129] Injection volume: 10μl;

[0130] Diluent: the mobile phase is n-hexane:isopropanol=99.5:0.5 (V:V).

[0131] 2. Experimental steps

[0132] (1)A 5 Reference substance solution stock solution: Accurately weigh A 5 100.18mg plus diluent dissolved to make 0.501mg / mLA 5 Reference substance solution stock solution;

[0133] (2)A 5 Positioning solution:: Precise measurement of A 5 Put 1.0ml of the stock solution of the reference substance solution in a 10 volumetric bottle, add diluent to the mark, shake well, and obtain;

[0134] (...

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Abstract

The invention belongs to the field of analytical chemistry, and particularly relates to a method for separating and determining a calcipotriene starting raw material A and related impurities. According to the method, elution is performed by using a silica gel as a stationary phase and using the mixed solution of n-hexane and isopropanol as a mobile phase. With the method of the present invention,the calcipotriene starting material A and the impurities thereof can be effectively separated; the separation determination can be performed by using high efficiency liquid chromatography, such that the effective separation can be achieved, and the contents of the calcipotriene starting material A and various impurities thereof can be accurately determined; and the method has advantages of strongspecificity and high sensitivity, and can provide the extremely important significance for the quality control and the safety assurance of the calcipotriene starting material A.

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 starting material A and related impurities. Background technique [0002] Calcipotriol is a derivative of vitamin D, which can inhibit the excessive proliferation of skin cells (keratinocytes) and induce their differentiation, so that the abnormal proliferation and differentiation of psoriatic skin cells can be corrected. local treatment. [0003] Compound A is an important starting material for the synthesis of calcipotriol, and its structural formula is as follows: [0004] [0005] In order to control the quality of the calcipotriol starting material A, it is necessary to separate and measure the calcipotriol starting material A and its impurities. Common impurities in calcipotriol starting material A are A 1 、A 2 、A 3 、A 4 and A 5 , and their structural formulas are shown in formula II, formula III, f...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/88
Inventor 杨婧周春燕夏爽
Owner CHONGQING HUABANGSHENGKAI PHARM