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High performance liquid chromatography (HPLC) determination method for related substances in difluprednate

A technology for difluprednate and related substances, which is applied in the field of drug analysis and detection to achieve the effects of improving reliability, strong practicability and simple operation

Active Publication Date: 2013-10-23
SHANDONG INST OF PHARMA IND
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  • Abstract
  • Description
  • Claims
  • Application Information

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  • High performance liquid chromatography (HPLC) determination method for related substances in difluprednate
  • High performance liquid chromatography (HPLC) determination method for related substances in difluprednate
  • High performance liquid chromatography (HPLC) determination method for related substances in difluprednate

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Embodiment 1

[0025] 1. Chromatographic conditions and system suitability test:

[0026] 1.1. Selection of chromatographic conditions:

[0027] Instrument: Shimadzu: LC-20AT, SPD-M20A, SIL-20A, DGU-20A5, the optimum column temperature is 35°C, and the flow rate is 1.0ml / min. The liquid chromatography column uses octadecylsilane bonded silica gel as the filler (250mm×4.6mm, 5μm). Referring to the relevant literature and combined with the specific conditions of the test, methanol-water, acetonitrile-water, methanol-water-glacial acetic acid were successively selected , methanol-acetonitrile-sodium acetate buffer solution and other conditions, and finally determined that the mobile phase is composed of acetate buffer (adjust the pH value to 3.5 with acetic acid)-acetonitrile-methanol, and its optimal ratio is (60:30 : 10). The injection volume is 10 μl.

[0028] Under this chromatographic condition, the retention time of the main peak of difluprednate is moderate, and the peak shape is...

Embodiment 2

[0038] Embodiment two, the determination of related substances of difluprednate ophthalmic emulsion

[0039] Take an appropriate amount of the content of this product, accurately measure (approximately equivalent to 5 mg of difluprednate), add mobile phase to prepare a solution containing 0.5 mg per 1 ml, filter, and take the filtrate as the test solution. Precisely measure an appropriate amount, add mobile phase to dilute to a solution containing about 5 μg per 1 ml, and use it as a control solution. Under the following selected chromatographic conditions: diode array detector (Shimadzu: LC-20AT, SPD-M20A, SIL-20A, DGU-20A5), using octadecylsilane bonded silica gel as filler, acetic acid Salt buffer (adjust the pH value to 3.5 with acetic acid)-acetonitrile-methanol (60:30:10) as the mobile phase, the column temperature is 35°C, and the flow rate is 1.0ml / min. Theoretical plate number should be not less than 3000 according to the calculation of difluprednate peak. Get cont...

Embodiment 3

[0042] Embodiment three: the determination of compound difluprednate eye drops related substances

[0043]Take appropriate amount of the content of this product, accurately measure (approximately equivalent to 5 mg of difluprednate), add mobile phase to prepare a solution containing 0.5 mg per 1 ml, filter, and take the filtrate as the test solution. Precisely measure an appropriate amount, add mobile phase to dilute to a solution containing about 5 μg per 1 ml, and use it as a control solution. Under the following selected chromatographic conditions: diode array detector (Shimadzu: LC-20AT, SPD-M20A, SIL-20A, DGU-20A5), using octadecylsilane bonded silica gel as filler, acetic acid Salt buffer (adjust the pH value to 3.5 with acetic acid)-acetonitrile-methanol (60:30:10) as the mobile phase, the column temperature is 35°C, and the flow rate is 1.0ml / min. Theoretical plate number should be not less than 3000 according to the calculation of difluprednate peak. Get contrast s...

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Abstract

The invention discloses a detection method of difluprednate. Specifically, the detection method adopts a diode array detector and takes an acetate buffer solution (with pH value regulated to 3.5 through acetic acid)-acetonitrile-methanol solution as a mobile phase. The method comprises the steps of preparing proper amounts of difluprednate and related preparations containing the difluprednate, adding the mobile phase to prepare a solution each 1ml of which contains 0.5mg of the difluprednate, and taking the prepared solution as a test solution; thinning the solution by the mobile phase to obtain a solution each 1ml of which contains about 5 micrograms, and taking the solution as a reference solution; and respectively introducing samples, wherein the sum of peak areas of various impurities in chromatogram of the test solution is not greater than main peak area of the reference solution. The method for detecting related substances of the difluprednate and related preparations containing the difluprednate can rapidly and accurately detect impurity and degradation product situations of the difluprednate; and the method is simple and convenient to operate, high in sensitivity, and capable of better controlling product quality.

Description

technical field [0001] The invention relates to a method for detecting related substances of difluprednate and related preparations containing difluprednate, belonging to the field of drug analysis and detection. Background technique [0002] Difluprednate is an ophthalmic anti-inflammatory drug, mainly used to treat local inflammation and pain after ophthalmic surgery. The chemical name is 6α, 9difluoro-11β, 17,21-trihydroxypregna-1,4-diene-3,20- dione 21-acetate 17butyrate. The structural formula is as follows: [0003] [0004] The molecular formula is: C 27 h 34 f 2 o 7 , Molecular weight: 508.5515, because difluprednate may introduce residual raw materials and other related substances during the synthesis process, and may also produce degradation products during storage, this method is effective for difluprednate after dissociation For purity analysis, this test uses a common chromatographic column (C 18 The chromatographic column) quickly and accurately reali...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 冯光玲冯爱国丁文娟孔祥雨刘宪华
Owner SHANDONG INST OF PHARMA IND
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