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Separation and detection method of isomer impurities in 3-halogenated-7-(4-bromobenzoyl)-1H-indole and application

A bromobenzoyl and detection method technology, which is applied in the field of separation and detection of isomer impurities in 3-halo-7--1hydro-indole, to improve safety and effectiveness, strong specificity, and separation good effect

Pending Publication Date: 2021-12-31
TIANJIN PHARMA GROUP CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the impurity and its detection method have not been reported in the literature.

Method used

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  • Separation and detection method of isomer impurities in 3-halogenated-7-(4-bromobenzoyl)-1H-indole and application
  • Separation and detection method of isomer impurities in 3-halogenated-7-(4-bromobenzoyl)-1H-indole and application
  • Separation and detection method of isomer impurities in 3-halogenated-7-(4-bromobenzoyl)-1H-indole and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Embodiment 1 specificity test

[0059] LD-Z1 reference substance solution: Accurately weigh an appropriate amount of LD-Z1 reference substance, dissolve and dilute with the sample solution to make a solution containing 0.4mg per 1mL, and use it as the LD-Z1 reference substance stock solution. Precisely measure 0.5mL of LD-Z1 reference substance stock solution, put it in a 100mL measuring bottle, dilute to the mark with sample solution, shake well, and use it as LD-Z1 reference substance solution.

[0060] Chlorinated reference substance solution: Accurately weigh an appropriate amount of chlorinated reference substance, dissolve and dilute the sample solution to make a solution containing 0.4 mg per 1 mL, and use it as a chlorinated reference substance stock solution. Precisely measure 1mL of the chlorinated substance reference substance stock solution, put it in a 100mL measuring bottle, dilute to the mark with the sample solution, shake well, and use it as the chlorin...

Embodiment 1-1

[0064] Chromatographic conditions:

[0065] Column: IA (4.6mm×250mm, 5μm);

[0066] Mobile phase: n-hexane-isopropanol is used as the mobile phase, and the volume ratio of the two is 95:5;

[0067] Detection wavelength: UV detector, the detection wavelength is 220nm;

[0068] Flow rate: 1.0mL / min;

[0069] Column temperature: 30°C;

[0070] Injection volume: 20μL;

[0071] Isocratic elution.

[0072] The HPLC spectrogram of LD-Z1 reference substance solution is as follows figure 1 shown.

[0073] Depend on figure 1 It can be seen that the retention time of LD-Z1 is 21.185min.

[0074] The HPLC spectrogram of chloride reference substance solution is as follows figure 2 shown.

[0075] Depend on figure 2 It can be seen that the retention time of chloride is 27.860min.

[0076] The HPLC spectrogram of LD-Z1+chloride mixed solution is as follows image 3 As shown, the detection data are shown in Table 1.

[0077] Table 1 Test results of LD-Z1+ chloride mixed solu...

Embodiment 1-2

[0081] Chromatographic conditions:

[0082] Column: IA (4.6mm×250mm, 5μm);

[0083] Mobile phase: n-hexane-isopropanol is used as the mobile phase, and the volume ratio of the two is 98:2;

[0084] Detection wavelength: UV detector, the detection wavelength is 215nm;

[0085] Flow rate: 1.1mL / min;

[0086] Column temperature: 35°C;

[0087] Injection volume: 20μL;

[0088] Isocratic elution.

[0089] The detection data of LD-Z1+ chloride mixed solution are shown in Table 2.

[0090] Table 2 Detection results of LD-Z1+ chloride mixed solution

[0091]

[0092]

[0093] It can be seen from Table 2 that the resolution between LD-Z1 and chlorinated compounds is greater than 2, which meets the requirements, and the detection method under the chromatographic conditions of the present invention can completely separate LD-Z1 and chlorinated compounds without mutual interference.

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Abstract

The invention provides a separation and detection method of isomer impurities in 3-halogenated-7-(4-bromobenzoyl)-1H-indole and application, and relates to the technical field of analytical chemistry. The method adopts high performance liquid chromatography, and the chromatographic conditions comprise: adopting a normal-phase chiral chromatographic column; an n-hexane-isopropanol mixed solution is used as a mobile phase; isocratic elution is performed; and the isomer impurity is 3-halogenated-7-(3-bromobenzoyl)-1-hydrogen-indole, and the structural formula of the isomer impurity is shown in the description. System methodology verifies that the method is good in system adaptability, high in specificity, good in durability and high in sensitivity, can be used for measuring and separating raw materials of the raw material medicine bromfenac sodium and isomer impurities of the raw materials, and improves the use safety and effectiveness of the bromfenac sodium eye drops.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to a method for separating and detecting isomer impurities in 3-halo-7-(4-bromobenzoyl)-1 hydrogen-indole and its application. Background technique [0002] Bromfenac sodium, whose chemical name is 2-amino-3-(4-bromobenzoyl) phenylacetate sodium, is a non-steroidal anti-inflammatory drug. Bromfenac sodium eye drops was first launched by Senju Company in Japan in 2000, and is used for the treatment of conjunctivitis, blepharitis, dynastic inflammation (comprising superior dynastic inflammation) and postoperative inflammation. [0003] At present, the mainstream synthesis method of bromfenac sodium is to use p-bromobenzonitrile and indoline as raw materials, use boron trichloride and aluminum trichloride as catalysts, carry out Friedel-crafts acylation, and then oxidize through active manganese dioxide , NBS or NCS halogenation, phosphoric acid hydrolysis, sodium hydroxi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/74G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/74G01N30/8675
Inventor 路起飞孔庆兰郑项元
Owner TIANJIN PHARMA GROUP CORP
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