Method for separating and determining diflucortolone as well as 6 beta diflucortolone and 16 beta diflucortolone thereof

A difluorometasone, stationary phase technology, applied in the field of analytical chemistry, to achieve the effect of good separation, excellent separation performance and durability, and strong specificity

Active Publication Date: 2018-06-29
CHONGQING HUAPONT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] At present, there is no public report on the relevant detection method, so the development of high performance liquid chromatography, using octylsilane bonded silica gel as a filler, durable, environmentally friendly, low toxicity and can quickly separate diflumethasone and its 6β diflumethasone and 16β The analysis method of diflumethasone is very meaningful for the health of pharmaceutical analysts and the quality control of their products and the study of degradation pathways

Method used

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  • Method for separating and determining diflucortolone as well as 6 beta diflucortolone and 16 beta diflucortolone thereof
  • Method for separating and determining diflucortolone as well as 6 beta diflucortolone and 16 beta diflucortolone thereof
  • Method for separating and determining diflucortolone as well as 6 beta diflucortolone and 16 beta diflucortolone thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] Example 1 Separation and Determination of Diflumethasone and 6β Diflumethasone and 16β Diflumethasone

[0074] The mobile phase that embodiment adopts and diluent are as follows:

[0075] mobile phase:

[0076] Mobile phase A: Inorganic salt buffer system Buffer salt: Weigh 3.7g of potassium hexafluorophosphate (0.02mol / L potassium hexafluorophosphate) into a 1000ml volumetric flask, add water to dissolve and dilute to the mark, adjust the pH value to 3.0± with phosphoric acid 0.1;

[0077] Mobile phase B: Methanol;

[0078] The volume ratio of mobile phase A and mobile phase B is 50:50.

[0079] Diluent: 50% methanol (methanol V: water V = 50:50).

[0080] 1) Sample dilution

[0081] 6β-diflumetasone: Take about 10 mg of 6β-diflumetasone reference substance, put it in a 100ml measuring bottle, add diluent to dissolve and dilute to the mark, and shake well to obtain 6β-diflumetasone stock solution.

[0082] 16β-diflumetasone: take about 10 mg of 16β-diflumetasone ...

Embodiment 2

[0088] Example 2 Basic research on detection limit and quantitative limit of diflumethasone, 6β diflumethasone and 16β diflumethasone by chromatographic system

[0089] Quantitation limit solution: Accurately weigh diflumethasone, 6β diflumethasone and 16β diflumethasone reference substances, make a solution with a certain concentration, and dilute step by step to obtain a quantification limit solution.

[0090] Detection limit solution: Precisely pipette 7.0ml of the limit of quantification solution, put it in a 20ml measuring bottle, add diluent to dilute to the mark, and shake well to obtain the limit of detection solution.

[0091] test methods:

[0092] The above quantification limit solution was continuously injected 3 times, and the detection limit solution was continuously injected 2 times, and the ratio of the main peak height to noise (signal-to-noise ratio) was calculated. Record the chromatogram ( image 3 ), the test results are shown in Table 2 and Table 3.

...

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Abstract

The invention belongs to the field of analytical chemistry, and concretely relates to a method for separating and determining diflucortolone as well as 6 beta diflucortolone and 16 beta diflucortolonethereof. A stationary phase adopted by the method is an octylsilanebonded silica gel. The method comprises the concrete steps of injecting a diflucortolone sample solution into a chromatographic instrument, adopting a mixed solution of a potassium hexafluorophosphatebuffer salt system and an organic solvent as a moving phase for eluting, and detecting in a detector. The method can be used for separating and content-determining of the diflucortolone as well as the 6 betadiflucortolone and the 16 beta diflucortolone thereof at the same time, achieves better effects on tailing factors and theoretical pedal number, has excellent separating property and durability, and is simple, convenient, feasible, good in reproducibility, efficient, fast, and high in specificity.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for separating and measuring diflumethasone, 6β diflumethasone and 16β diflumethasone by high performance liquid chromatography and an application thereof. Background technique [0002] Flumethasone (Flumethasone) was listed in the United States in 1998. It is a moderate-strength topical steroid drug and a synthetic difluoroglucocorticoid with anti-inflammatory, vasoconstrictive and anti-proliferative effects. The introduction of the trimethyl acetate group at the C-21 position makes it difficult for diflumethasone to be absorbed through the skin, which leads to the fact that diflumethasone can produce a drug effect at a very low concentration. Noninfectious inflammatory skin diseases that respond to corticosteroid therapy, especially those associated with hyperkeratosis, such as: seborrheic dermatitis, contact dermatitis, atopic dermatitis, localized neur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 林晓兵易光明
Owner CHONGQING HUAPONT PHARMA
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