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Method for measuring chromatographic purity of difluprednate

A technology for difluprednate and a determination method, which is applied in the directions of measuring devices, instruments, scientific instruments, etc., can solve the problems of complicated mobile phase preparation, unsatisfactory separation effect, low number of theoretical plates, etc., and achieves ideal separation effect, Good peak shape, simple preparation effect

Inactive Publication Date: 2017-10-27
广州仁恒医药科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Disadvantages: The main peak of this method emerges late, and the separation effect is not ideal
Disadvantages: This method has poor peak shape and low theoretical plate number
Disadvantages: This method is complicated to prepare the mobile phase and takes a long time
[0007] The chromatographic purity assay method of present difluprednate all has deficiencies and needs to be improved

Method used

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  • Method for measuring chromatographic purity of difluprednate
  • Method for measuring chromatographic purity of difluprednate
  • Method for measuring chromatographic purity of difluprednate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Instrument: Waters 2695 (2487 ​​ultraviolet-visible light detector, Empower 3 chromatographic workstation), accurately measure 15 μ L of the test solution and inject it into the chromatograph, using methanol-water ratio of 68:32 as mobile phase, flow rate of 0.9ml / min, detection The wavelength is 240nm, record the chromatogram to 2 times the retention time of the main peak of difluprednate, and calculate the chromatographic purity by adjusting the appropriate instrument integration parameters and the area normalization method. The detection result shows that under this chromatographic condition, the peak eluting time of difluprednate is moderate, about 25min, the peak shape is good, see the attached figure 1 , the resolution is 20.56, see attached figure 2 . And when using methanol-water (50:50) as the mobile phase, there is no peak within 60min, the main peak will appear in the next sample, and its baseline is unstable, fluctuating from time to time, and the peak sha...

Embodiment 2

[0035] Precisely measure 15 μL of the test solution and inject it into the chromatograph, select the following chromatographic conditions for detection: use a C18 chromatographic column, column temperature 35 ° C, methanol-water ratio of 68:32 as mobile phase, flow rate of 1.0ml / min, The detection wavelength is 240nm, and the chromatogram is recorded to 2 times the retention time of the main peak of difluprednate, and the chromatographic purity is calculated by adjusting the appropriate instrument integration parameters and the area normalization method. The detection result shows that under this chromatographic condition, the peak time of difluprednate is moderate, and the peak shape is good, see the attached Figure 4 , good resolution, see attached Figure 5 .

Embodiment 3

[0037] Accurately measure 15 μ L of the test solution and inject it into the chromatograph, select the following chromatographic conditions for detection: adopt a C18 chromatographic column, column temperature 35°C, methanol-water (60:40) as mobile phase, flow rate of 1.0ml / min, The detection wavelength is 240nm, and the chromatogram is recorded to 2 times the retention time of the main peak of difluprednate, and the chromatographic purity is calculated by adjusting the appropriate instrument integration parameters and the area normalization method. The detection result shows that under this chromatographic condition, the peak time of difluprednate is moderate, and the peak shape is good, see the attached Image 6 , good resolution, see attached Figure 7 .

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Abstract

The invention discloses a method for measuring chromatographic purity of difluprednate. The method comprises the following steps: 1, preparation: chromatographic conditions: an ultraviolet visible light detector and an ultimate XB-C18 chromatographic column are adopted, the detection wavelength is 240 nm, the column temperature is 35 DEG C, the flow velocity is 0.9 ml / min, the flowing phase is that the methanol / water ratio is 68:32, and the sampling quantity is 15 [mu]L; preparation of a sample-for-test liquid: taking a proper amount of difluprednate, and adding a flowing phase to prepare a solution of 5 mg / ml to serve as the sample-for-test solution; step 2, purity measurement: injecting the sample-for-test solution into a chromatographic instrument, recording a chromatogram till twice retention time of a difluprednate main peak is reached, adjusting a proper instrument integral parameter and calculating by using an area normalization method to obtain the chromatographic purity. Compared with the prior art, the method for measuring the chromatographic purity of the difluprednate has the advantages of being simple and accurate, high in sensitivity and capable of effectively detecting the purity of the difluprednate.

Description

technical field [0001] The invention relates to the field of substance purity determination, in particular to a chromatographic purity determination method of difluprednate. Background technique [0002] Difluprednate is also known as difluprednate or defluprednate, and its ophthalmic emulsion trade name is "Durezol", which was researched and developed by Sirion Therapeutics and passed priority approval on June 23, 2008 The procedure is FDA-approved. This medicine is an ophthalmic medicine used topically to treat inflammation and pain after eye surgery. Difluprednate is an adrenocortical hormone drug, a difluoro derivative of prednisolone, which has strong anti-inflammatory and analgesic effects, and can inhibit inflammation-related edema, cellulose deposition, telangiectasia, leukocyte Migration, capillary proliferation, fibroblast proliferation, collagen deposition, and scar formation. Its chemical name is 6α, 9α-fluoro-11β-hydroxy-4-ene-pregna-3, 20-diketone-17-butyrat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 田元周胜安覃宇东邓琦李金霞许志国
Owner 广州仁恒医药科技股份有限公司
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