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Method for measuring phenylhydrazine compound residues in crude drugs through HPLC (high performance liquid chromatography)

A technology for compounds and APIs, applied in the field of pharmaceutical analysis

Active Publication Date: 2013-12-18
WATERSTONE PHARMA WUHAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In the prior art, the detection sensitivity of phenylhydrazine in the patent CN102841170A that China has applied for is 0.01% (100ppm), and in the Chinese Pharmacopoeia analysis method of phenylhydrazine, the detection sensitivity is 0.05% (500ppm) and this method is only applicable to phenylhydrazine detection

Method used

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  • Method for measuring phenylhydrazine compound residues in crude drugs through HPLC (high performance liquid chromatography)
  • Method for measuring phenylhydrazine compound residues in crude drugs through HPLC (high performance liquid chromatography)
  • Method for measuring phenylhydrazine compound residues in crude drugs through HPLC (high performance liquid chromatography)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Instrument: Agilent1260 high performance liquid chromatography, 1260 ultraviolet detector

[0042] Chromatographic column: chromatographic column with phenyl bonded silica gel as filler (250×4.6mm, 5μm);

[0043] Mobile phase A: 0.01mol / L ammonium acetate buffer (pH5.1)

[0044] Mobile Phase B: Acetonitrile

[0045] See the table below for gradient elution;

[0046] time (min)

Mobile Phase A(%)

Mobile phase B(%)

0

90

10

3

90

10

14

80

20

15

10

90

25

10

90

30

90

10

35

90

10

[0047] Flow rate: 1.0mL / min

[0048] Detection wavelength: 260nm

[0049] Column temperature: 30°C

[0050] Injection volume: 10μL

[0051] Diluent: Methanol

[0052] experiment procedure:

[0053] Need test solution: Weigh 1.0014g of celecoxib sample, put it in a 10mL measuring bottle, dissolve it with diluent and dilute to the mark, shake well.

[0054] Reference s...

Embodiment 2

[0058] Instrument: Agilent1260 high performance liquid chromatography, 1260 ultraviolet detector

[0059] Chromatographic column: chromatographic column with phenyl bonded silica gel as filler (250×4.6mm, 5μm);

[0060] Mobile phase A: 0.02mol / L ammonium acetate buffer (pH4.9)

[0061] Mobile Phase B: Acetonitrile

[0062] See the table below for gradient elution;

[0063] time (min)

Mobile Phase A(%)

Mobile phase B(%)

0

90

10

3

90

10

14

80

20

15

10

90

25

10

90

30

90

10

35

90

10

[0064] Flow rate: 1.0mL / min

[0065] Detection wavelength: 260nm

[0066] Column temperature: 25°C

[0067] Injection volume: 10μL

[0068] Diluent: Methanol

[0069] experiment procedure:

[0070] Reference substance solution: Accurately weigh 37.48mg of p-hydrazinobenzenesulfonamide hydrochloride reference substance, put it in a 100mL measuring bottle, dissolve it...

Embodiment 3

[0075] Instrument: Agilent1260 high performance liquid chromatography, 1260 ultraviolet detector

[0076] Chromatographic column: chromatographic column with phenyl bonded silica gel as filler (250×4.6mm, 5μm);

[0077] Mobile phase A: 0.01mol / L ammonium acetate buffer (pH3.0)

[0078] Mobile Phase B: Acetonitrile

[0079] See the table below for gradient elution;

[0080] time (min)

Mobile Phase A(%)

Mobile phase B(%)

0

90

10

3

90

10

14

80

20

15

10

90

25

10

90

30

90

10

35

90

10

[0081] Flow rate: 1.0mL / min

[0082] Detection wavelength: 260nm

[0083] Column temperature: 25°C

[0084] Injection volume: 20μL

[0085] Diluent: Acetonitrile

[0086] experiment procedure:

[0087] The test solution: Weigh 0.50261 g of the crude product of deferasirox, put it in a 10 mL measuring bottle, dissolve it with a diluent and dilute to the mark, and sha...

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Abstract

The invention discloses a method for measuring genotoxic impurities (or doubtful genotoxicity), namely phenylhydrazine compound residues, in crude drugs through the HPLC (high performance liquid chromatography). The detection is directly implemented by taking phenyl bonded silica gel as a chromatographic column of a solid phase and organic phase and buffer solution mixed solvent gradient elution as a mobile phase. The detection method is high in detection sensitivity, strong in specificity, high in precision, high in accuracy, convenient to operate and strong in adaptability and can be used for detecting phenylhydrazine compounds in various crude drugs, and the quality of the crude drugs can be effectively controlled.

Description

technical field [0001] The invention belongs to the field of drug analysis, and in particular relates to a method for determining residues of phenylhydrazine compounds in raw materials by using HPLC (high performance liquid chromatography). Background technique [0002] In drug synthesis, phenylhydrazine compounds are often used as the starting / key materials of various active pharmaceutical ingredients (API, Active Pharmaceutical Ingredient), but due to their genotoxicity (or suspected genotoxicity), the European Union has published phenylhydrazine compounds As a genotoxic impurity (or suspected genotoxic impurity), it is required to strictly control the relevant substances in the raw material drug, and the maximum daily dose prescribed by the EU is 1.5 μg. [0003] The structural formula of phenylhydrazine compounds is as follows, R represents sulfonamide group, carboxyl group, hydrogen atom, methanesulfonyl group and the like. [0004] [0005] The following describes ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 夏艳开
Owner WATERSTONE PHARMA WUHAN
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