Separation and determination methods for dapoxetine hydrochloride intermediate SM1 and related impurities

A technology for dapoxetine hydrochloride and intermediates, applied in the field of analytical chemistry, can solve the problem of not separating SM1 and related impurities SM1 and related impurities, and achieve effective control, accurate measurement, and separation

Active Publication Date: 2016-10-05
CHONGQING HUAPONT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no method for separating SM1 and related impuri...

Method used

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  • Separation and determination methods for dapoxetine hydrochloride intermediate SM1 and related impurities
  • Separation and determination methods for dapoxetine hydrochloride intermediate SM1 and related impurities
  • Separation and determination methods for dapoxetine hydrochloride intermediate SM1 and related impurities

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] Example 1 The positioning of dapoxetine hydrochloride intermediate SM1 and related impurities 3-chloropropiophenone, propiophenone, 1-phenylpropanol, naphthol, SM1a, SM1b, SM1c, SM1d, SM1e and UI-1

[0075] (1) Preparation of positioning solutions for SM1 and impurities 3-chloropropiophenone, propiophenone, 1-phenylpropanol, naphthol, SM1a, SM1b, SM1c, SM1d, SM1e and UI-1

[0076] Preparation of 3-chloropropiophenone positioning solution: Weigh 10.55 mg of 3-chloropropiophenone, put it in a 50ml volumetric flask, add diluent to dissolve and dilute to the mark, shake well, and use it as impurity 3-chloropropiophenone stock solution; Take 1.0ml of the above-mentioned 3-chloropropiophenone stock solution, put it in a 100ml volumetric flask, add diluent to dilute to the mark, and shake well to obtain the 3-chloropropiophenone positioning solution with a concentration of 2.11 μg / ml.

[0077]Propiophenone positioning solution: Weigh 12.40mg of propiophenone, put it in a 25ml ...

Embodiment 2

[0089] Example 2 Separation of dapoxetine hydrochloride intermediate SM1, 3-chloropropiophenone, propiophenone, 1-phenylpropanol, naphthol, SM1a, SM1b, SM1c, SM1d, SM1e and UI-1

[0090] (1) Preparation of mixed solutions of SM1, 3-chloropropiophenone, propiophenone, 1-phenylpropanol, naphthol, SM1a, SM1b, SM1c, SM1d, SM1e and UI-1

[0091] Accurately pipette the SM prepared in Example 1 1a , SM 1b , SM 1c , SM 1d 1.0ml of each stock solution, 6.0ml each of SM1, 3-chloropropiophenone, propiophenone, 1-phenylpropanol, naphthol, SM1e and UI-1 stock solution, put them in the same 100ml volumetric flask, add diluent to dilute to scale, shake well, that is a mixed solution.

[0092] (2) With 45% acetonitrile aqueous solution (acetonitrile: water=45:55) as mobile phase, get the mixed solution that makes and analyze according to above-mentioned chromatographic conditions, record chromatogram as follows Figure 12 Shown, it can be seen that the method SM1 of the present invention...

Embodiment 3

[0093] Separation and detection of SM1, 3-chloropropiophenone, propiophenone, 1-phenylpropanol, naphthol, SM1a, SM1b, SM1c, SM1d, SM1e and UI-1 in the test sample

[0094] (1) Preparation of the test product solution: Take about 25 mg of the test product and dissolve it with a diluent to make a 0.5 mg / mL test solution.

[0095] (2) Self-contrast solution: Precisely pipette 0.5ml of the test solution prepared in step (1), put it in a 100ml volumetric flask, add diluent to dilute 200 times, and prepare a 0.0025mg / mL self-contrast solution.

[0096] (3) The mobile phase, acetonitrile aqueous solution, was subjected to gradient elution according to the elution conditions shown in Table 1.

[0097] Table 1 Gradient elution table (volume ratio of acetonitrile and water)

[0098] time (min)

Acetonitrile

water

0

45

55

13

45

55

25

70

30

30

85

15

38

85

15

38.01

45

55

45

45

55

...

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Abstract

The invention specifically relates to separation and determination methods for a dapoxetine hydrochloride intermediate SM1 and related impurities, belonging to the field of analytical chemistry. The separation method employs octadecyl bonded porous silica gel and/or inorganic oxide particles as a stationary phase and an aqueous acetonitrile solution as a mobile phase for separation, and can realize effective separation of SM1 and related impurities. The determination method employs high performance liquid chromatography and comprises the following steps: preparing a test solution from a test sample; diluting the test solution by certain times so as to obtain a contrast solution; analyzing the test solution and the contrast solution by using the stationary phase and the mobile phase; recording a chromatogram; and calculating the contents of SM1 and related impurities in the test sample by using a main component self-contrast method. The separation and determination methods can realize effective separation of SM1 and related impurities and accurately measure the contents of SM1 and related impurities, and are simple to operate and high in accuracy.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for separating and measuring dapoxetine hydrochloride intermediate SM1 and related impurities. Background technique [0002] Dapoxetine Hydrochloride (Dapoxetine Hydrochloride), chemical name S-(+)-N,N-dimethyl-1-phenyl-3-(1-naphthyloxy)propylamine hydrochloride (S-(+) -N,N-dimethyl-3-(naphthalene-1-yloxy)-1-phenylpropan-1-amine Hydrochloride), is the hydrochloride of dapoxetine, and the original manufacturer of dapoxetine is Eli Lili Company of the United States , whose original patent EP 0288188 describes the preparation of dapoxetine. Dapoxetine hydrochloride is a selective serotonin reuptake inhibitor (SSRI), which is a short-acting SSRI. Compared with the traditional long-acting SSRI, it has the characteristics of fast drug effect, short half-life, and low side effects. For the treatment of depression and related affective disorders. Dapoxetine hyd...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/02
Inventor 曾正英谢文丽
Owner CHONGQING HUAPONT PHARMA
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