Method for extracting compounds with pregnane mother nucleus structure from compositions

A composition and compound technology, applied in the field of analytical chemistry, can solve the problems of high noise, interference, inaccuracy, etc., and achieve the effect of clean baseline, stable sample solution and high number of theoretical plates.

Active Publication Date: 2014-12-10
CHONGQING HUAPONT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing literature, only the main drug in the sample is dissolved and the content is determined, and the influence of the dissolved matrix on the determination is not paid much attention to

Method used

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  • Method for extracting compounds with pregnane mother nucleus structure from compositions
  • Method for extracting compounds with pregnane mother nucleus structure from compositions
  • Method for extracting compounds with pregnane mother nucleus structure from compositions

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080] Embodiment 1 Determination of related substances in halometasone cream

[0081] (1) Chromatographic method

[0082] Chromatographic column: Shimpack VP-ODS (250mm×4.6mm, 5μm)

[0083] UV detector: 254nm

[0084] Column temperature: 25°C

[0085] Flow rate: 1.5ml / min

[0086] Injection volume: 20μl

[0087] System suitability: The resolution of Halometapine peak and adjacent impurity peak should reach 1.5.

[0088] Mobile phase: Phase A is 0.1% glacial acetic acid solution, phase B is acetonitrile, and the gradient elution is performed as follows:

[0089]

[0090] (2) Extraction and testing

[0091] Get about 10 g of the content of halometasone cream (produced by Chongqing Huabang Pharmaceutical Co., Ltd., specification 0.05%) (approximately equivalent to halometasone 5 mg), put it in a stoppered Erlenmeyer flask, add 10 ml of acetonitrile and 0.2 g of sodium chloride, 60 ℃ water bath to dissolve, put it in an ice-water bath for 30 minutes, take it out and sha...

Embodiment 2

[0099] Embodiment 2 Determination of related substances in clobetasone butyrate cream

[0100] (1) Chromatographic method

[0101] Chromatographic column: YMC-Pack ODS-A 150mm×4.6mm, 3.0μm

[0102] Flow rate: 1.5ml / min Column temperature: 40°C

[0103] Detection wavelength: 241nm

[0104] Injection volume: 30μl

[0105] Mobile phase: Phase A of the mobile phase is water, phase B is acetonitrile, and the gradient elution is performed as follows:

[0106]

[0107] (2) Extraction and testing

[0108] To operate in the dark, take an appropriate amount of clobetasone butyrate cream (produced by Sino-US Tianjin SmithKline Pharmaceutical Co., Ltd., specification 0.05%) (approximately equivalent to clobetasone butyrate 10mg), and put it in a stoppered Erlenmeyer bottle Add 16ml of acetonitrile and 0.2g of potassium chloride, dissolve in a water bath at 60°C, place in an ice bath for 60 minutes, take out and shake well, then place in a centrifuge, centrifuge at 4000rpm for 10 m...

Embodiment 3

[0117] Example 3 Determination of related substances in betamethasone dipropionate cream

[0118] (1) Chromatographic method

[0119] Chromatographic column: Agilent XDB-C18 (250mm×4.6mm, 5μm)

[0120] UV detector: 240nm

[0121] Column temperature: 25°C

[0122] Flow rate: 1.5ml / min

[0123] Injection volume: 20μl

[0124] Mobile phase: 45% acetonitrile

[0125] (2) Extraction and testing

[0126] Take about 10 g of the content of betamethasone dipropionate cream (produced by Chongqing Huabang Pharmaceutical Co., Ltd., specification 0.1%) (approximately equivalent to 10 mg of betamethasone dipropionate), put it in a stoppered Erlenmeyer flask, add 10 ml of acetonitrile and sodium chloride 0.2g, dissolved in a water bath at 60°C, placed in an ice-water bath for 30 minutes, taken out and shaken evenly, allowed to cool to room temperature, filtered the clear solution, and took the subsequent filtrate as the test solution. Precisely measure 1.0ml of the test solution, put ...

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Abstract

The invention particularly relates to a method for extracting compounds with a pregnane mother nucleus structure from compositions, belonging to the technical field of analytical chemistry. According to the method, inorganic salt is added into acetonitrile or an acetonitrile water solution which serves as a basic solvent so as to improve oil-water partition coefficients, the temperature is lowered to accelerate separation of auxiliary materials/matrixes in the compositions, and the separation of immiscible components such as oil and water is accelerated by centrifugation. The method has the beneficial effects that the universality is wide, the compounds can be effectively extracted without being damaged, and the subsequent analysis and detection cannot be interfered by the used solvent; the obtained solution can be directly utilized for carrying out high performance liquid phase analysis, and an obtained atlas has clean base lines, symmetric peak shapes and high number of theoretical plates; meanwhile, a sample solution is relatively stable, and more related substances can be detected; the method can be widely applied to the quality control of the compositions containing adrenocortical hormone components.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a method for extracting a compound with a pregnane core structure from a composition. Background technique [0002] Adrenal cortex hormones are steroidal hormones synthesized and secreted by the adrenal cortex and have a pregnane nucleus. Dozens of sterol crystals can be extracted from the adrenal cortex. The main function of this kind of compound is to regulate water-salt metabolism and sugar metabolism in animals, and it is ubiquitous in various vertebrates. About 30 adrenocortical hormones have been isolated and identified, about 10 of which are biologically active. Cortisol has the strongest activity and has the function of regulating sugar, protein and fat metabolism, which can affect the synthesis and utilization of glucose, mobilization of fat and protein synthesis. At present, the application of adrenal cortex hormones in drugs mainly includes ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 周维兰昌云颜波张吉谭辉
Owner CHONGQING HUAPONT PHARMA
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