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Detection method of brexpiprazole-related substance(s)

A detection method, the technology of ebiprazole, applied in the field of high performance liquid chromatography analysis, can solve the problems of fast ebiprazole peak time and inability to separate ebiprazole, and achieve simple and convenient detection method, high sensitivity, good repeatability

Active Publication Date: 2019-02-05
四川弘远药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] Since aripiprazole is similar in structure to ebiprazole, the inventor also tried to refer to the quality standard of aripiprazole in the second part of the Chinese Pharmacopoeia 2015 edition and the method in the import registration standard of aripiprazole raw material drug to treat ebipiprazole. However, the results showed that the ebiprazole peak time was too fast, and the ebiprazole impurities, ebiprazole and adjacent impurities could not be separated
Indicates that quality control methods for aripiprazole do not apply to ebiprazole

Method used

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  • Detection method of brexpiprazole-related substance(s)
  • Detection method of brexpiprazole-related substance(s)
  • Detection method of brexpiprazole-related substance(s)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0133] 1. Sample preparation

[0134] Impurity localization solution: appropriate amount of BPZ-impurity reference substance, put them in measuring bottles respectively, dissolve with methanol and dilute to the mark to get ready.

[0135] Table 6. BPZ-impurity concentration

[0136]

[0137] Sample solution: BPZ (151101) 11.32mg, put in a 50ml measuring bottle, dissolve with methanol and dilute to the mark.

[0138] Sample plus impurity control solution: Take the sample solution and add 50 μl of impurity localization solution.

[0139] Blank: Methanol

[0140] Note: BPZ-Impurity II preparation: dissolve and dilute to volume with dimethyl sulfoxide.

[0141] Preparation of BPZ-Impurity VII: Dissolve and dilute to volume with N,N dimethylformamide.

[0142] 2. Detection

[0143] Use octadecylsilane bonded silica gel as filler (5μm, 250*4.6mm); use acetonitrile as mobile phase A, pH value is 6.7, concentration is 0.02mol / L NaH 2 PO 4 Buffer-Acetonitrile (90:10) is the m...

Embodiment 2

[0151] 1. Sample preparation

[0152] With comparative example 1.

[0153] 2. Detection

[0154] Use octadecylsilane bonded silica gel as filler (5μm, 250*4.6mm); flow rate is 1.0ml per minute; column temperature is 35°C; detection wavelength is 254nm; phosphate is 0.02mol / L NaH 2 PO4 buffer, other conditions are as follows:

[0155] Table 8. Some HPLC chromatographic conditions

[0156]

[0157] Measure 50 μl of the solution and inject it into the liquid chromatograph for elution according to the following conditions:

[0158]

[0159]

[0160] 3. Results

[0161] The results under the detection conditions of experiment numbers 1-4 are as follows Figure 14 , 15 , 13, and 16. In the pH range of the buffer solution from 6.5 to 6.9, the separation between ebiprazole and adjacent impurities, as well as between each impurity, is greater than 1.5; the separation between ebiprazole and adjacent impurity peaks decreases as the pH value decreases, When the pH value i...

Embodiment 3

[0163] 1. Sample preparation

[0164] With comparative example 1.

[0165] 2. Detection

[0166] Use octadecylsilane bonded silica gel as filler (5μm, 250*4.6mm); mobile phase A is acetonitrile, mobile phase B is 0.02mol / L NaH without or containing a certain proportion of acetonitrile 2 PO4 buffer; the flow rate is 1.0ml per minute; the column temperature is 35°C; the detection wavelength is 254nm; the ratio of acetonitrile is as follows:

[0167] Table 9. Some HPLC chromatographic conditions

[0168]

[0169] Measure 50 μl of the solution and inject it into the liquid chromatograph for elution according to the following conditions:

[0170] time min

Mobile phase A%

Mobile phase B%

0

25

75

55

70

30

85

70

30

85.01

25

75

90

25

75

[0171] 3. Results

[0172] Carry out high-performance liquid chromatography detection according to above-mentioned condition, number is the experimental result u...

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Abstract

The present invention provides a detection method of brexpiprazole-related substance(s). The detection of the related substances is performed via a high performance liquid chromatography method. The determination condition of the liquid chromatography is: an octadecyl silane bonded silica gel is taken as a filler of a chromatographic column, a mobile phase A is acetonitrile, a mobile phase B is phosphate buffer-acetonitrile, and the detection is performed by adopting gradient elution. The method has the advantages of specificity, durability, good reproducibility and high sensitivity, and the method is suitable for the qualitative and quantitative detection of the brexpiprazole-related substance(s).

Description

technical field [0001] The invention relates to a high-performance liquid chromatography analysis method, in particular to a method for separating and analyzing ebiprazole-related substances by using high-performance liquid chromatography. Background technique [0002] Ebiprazole is the first dopamine, partial 5-HT1A receptor agonist and 5-HT2A receptor antagonist compound developed by Otsuka Pharmaceutical Company, and later jointly developed with Denmark Lundbeck Pharmaceuticals. Best-selling drug - another blockbuster after aripiprazole. Compared with aripiprazole, this product shows higher affinity to dopamine D2 receptor, 5-HT2A receptor and 5-HT1A receptor, but relatively lower affinity to H1 and M1 receptor. This product submitted a new drug application to the US FDA on July 14, 2014, and was approved for marketing on July 10, 2015. It is indicated for the adjuvant treatment of severe depression and the treatment of schizophrenia. The chemical name of ebiprazole is ...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 柯潇张伟
Owner 四川弘远药业有限公司
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