Separation and determination method of calcipotriol starting material a and related impurities

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

Active Publication Date: 2022-02-01
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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  • Separation and determination method of calcipotriol starting material a and related impurities
  • Separation and determination method of calcipotriol starting material a and related impurities
  • Separation and determination method of calcipotriol starting material a and related impurities

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] 1. Instruments and conditions

[0072] Instrument: high performance liquid chromatography;

[0073] Chromatographic column: Agilent ZORBAX SIL (4.6×250mm, 5μm);

[0074] Mobile phase: n-hexane:isopropanol=90:10(V:V);

[0075] UV detector detection wavelength: 200nm;

[0076] Column temperature: 30°C;

[0077] Flow rate: 1.0ml / min;

[0078] Injection volume: 10μl;

[0079] Diluent: The mobile phase is n-hexane:isopropanol=90:10 (V:V).

[0080] 2. Experimental steps

[0081] (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;

[0082] (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;

[0083] (3)A 3 Reference substance solution stock solution: Accurately weigh A 3 101.27mg plus diluent dissolved to make 5.06mg / mL A 3 ...

Embodiment 2

[0091] 1. Instruments and conditions

[0092] Instrument: high performance liquid chromatography;

[0093] Chromatographic column: Agilent ZORBAX SIL (4.6×250mm, 5μm);

[0094] Mobile phase: n-hexane:isopropanol=95:5(V:V);

[0095] Evaporative photodetector conditions: drift tube temperature: 51.0°C;

[0096] Gas flow rate: 1.7L / min;

[0097] Air pressure: 0.5Mpa;

[0098] Column temperature: 30°C;

[0099] Flow rate: 1.0ml / min;

[0100] Injection volume: 10μl;

[0101] Diluent: The mobile phase is n-hexane:isopropanol=95:5 (V:V).

[0102] 2. Experimental steps

[0103] (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;

[0104] (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;

[0105] ...

Embodiment 3

[0119] 1. Instruments and conditions

[0120] Instrument: high performance liquid chromatography;

[0121] Chromatographic column: Agilent ZORBAX SIL (4.6×250mm, 5μm);

[0122] Mobile phase: n-hexane:isopropanol=99.5:0.5(V:V);

[0123] Evaporative photodetector conditions: drift tube temperature: 42°C;

[0124] Gas flow rate: 1.7L / min;

[0125] Air pressure: 0.5Mpa;

[0126] Column temperature: 30°C;

[0127] Flow rate: 1.0ml / min;

[0128] Injection volume: 10μl;

[0129] Diluent: the mobile phase is n-hexane:isopropanol=99.5:0.5 (V:V).

[0130] 2. Experimental steps

[0131] (1)A 5 Reference substance solution stock solution: Accurately weigh A 5 100.18mg plus diluent dissolved to make 0.501mg / mL A 5 Reference substance solution stock solution;

[0132] (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° measuring bottle, add diluent to the mark, shake well, and obtain;

[0133] (...

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Abstract

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. The method uses silica gel as the stationary phase and elutes with a mixture of n-hexane and isopropanol as the mobile phase. This method can effectively separate the calcipotriol starting material A and its impurities. The method can also use high-efficiency Liquid chromatography is used for separation and determination, not only to achieve effective separation, but also to accurately determine the content of calcipotriol starting material A and its impurities, with strong specificity and high sensitivity. Quality control and safety assurance are of great significance.

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 calcipotriol starting material A, it is necessary to separate and measure calcipotriol starting material A and impurities thereof. 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, form...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/88
Inventor 杨婧周春燕夏爽
Owner CHONGQING HUABANGSHENGKAI PHARM
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