High performance liquid chromatography detection method for related substances in dapoxetine

A related substance, dapoxetine technology, applied in the field of drug analysis and detection, can solve problems such as high-performance liquid chromatography determination methods that have not yet been retrieved, and achieve the effects of improving reliability, strong practicability, and simple operation

Active Publication Date: 2014-07-16
SHANDONG INST OF PHARMA IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is currently no search for a method for the determination of dapoxetine and its related substances by high performance liquid chromatography

Method used

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  • High performance liquid chromatography detection method for related substances in dapoxetine
  • High performance liquid chromatography detection method for related substances in dapoxetine
  • High performance liquid chromatography detection method for related substances in dapoxetine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1. Chromatographic conditions and system suitability test:

[0025] 1.1. Selection of chromatographic conditions:

[0026] Instrument: Shimadzu: LC-20AT, SPD-M20A, SIL-20A, DGU-20A5, the optimum column temperature is 30°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-phosphate buffer solution and other conditions, and finally determined that the mobile phase is composed of phosphate buffer (adjust the pH value to 3.2 with phosphoric acid)-acetonitrile-methanol, and its optimal ratio is (40:30: 30). The injection volume is 10 μl.

[0027] Under the chromatographic conditions, the main peak of dapoxetine had a moderate retention time and a good peak shape.

[00...

Embodiment 2

[0037] Embodiment two, the mensuration of dapoxetine tablet related substance

[0038] Take 20 tablets of this product, accurately weigh them, grind them finely, and accurately weigh an appropriate amount (approximately equivalent to 2 mg of dapoxetine),

[0039] Add mobile phase to prepare a solution containing 0.2mg per 1ml, filter, and take the filtrate as the test solution. Precisely measure an appropriate amount, add mobile phase to dilute to a solution containing about 2 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, phosphate Buffer (adjust the pH value to 3.2 with phosphoric acid)-acetonitrile-methanol (40:30:30) as the mobile phase, the column temperature is 30°C, and the flow rate is 1.0ml / min. The number of theoretical plates should be no less than 3000 according to the Dapoxetine peak....

Embodiment 3

[0041] Embodiment Three: Determination of Related Substances in Dapoxetine Capsules

[0042]Take an appropriate amount of the content of this product, grind it finely, accurately weigh the fine powder (approximately equivalent to 2 mg of dapoxetine), add mobile phase to prepare a solution containing 0.2 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 2 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, phosphate Buffer (adjust the pH value to 3.2 with phosphoric acid)-acetonitrile-methanol (40:30:30) as the mobile phase, the column temperature is 30°C, and the flow rate is 1.0ml / min. The number of theoretical plates should be no less than 3000 according to the Dapoxetine peak. Take 10 μ...

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Abstract

The invention discloses a dapoxetine detection method using a diode array detector and using a phosphate buffer solution (pH value is adjusted to 3.2 with phosphoric acid)-acetonitrile-methanol solution as a mobile phase. The dapoxetine detection method is as follows: taking proper amounts of dapoxetine and dapoxetine-containing relevant preparations, adding the mobile phase to prepare a solution containing 0.2mg of the dapoxetine every 1ml of the solution as a solution to be tested; diluting the solution to be tested with the mobile phase into a solution containing 0.2mug of the dapoxetine every 1ml of the solution as a contrast solution; and respectively injecting samples; wherein the sum of peak areas of impurities in a chromatogram map of the solution to be tested may not be greater than main peak area of the contrast solution. According to the detection method for the related substances in the dapoxetine and the dapoxetine-containing relevant preparations, the conditions of the impurities and degradation products of the dapoxetine can be quickly and accurately detected, and the detection method is simple in operation and high in sensitivity, and can be used to better control the quality of the product.

Description

technical field [0001] The invention relates to a method for detecting related substances of dapoxetine and related preparations containing dapoxetine, belonging to the field of drug analysis and detection. Background technique [0002] Dapoxetine (INN, trade name Priligy), is the world's first drug to prevent premature ejaculation. The chemical name is (S)-N,N-dimethyl-3-(naphthalen-1-yloxy)-1-phenylpropan-1-amine, and the structural formula is as follows: . [0003] The molecular formula is: C 21 h 23 NO, molecular weight: 305.413, since dapoxetine may introduce residual raw materials and other related substances during the synthesis process, and may produce degradation products during storage, this method is effective for the purity analysis of dapoxetine. The test uses a common chromatographic column (C 18 Chromatographic column) quickly and accurately realize the determination of related substances of dapoxetine and ensure the quality control of dapoxetine. [00...

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冀东付丙月
Owner SHANDONG INST OF PHARMA IND
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