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Method for determining genotoxic impurities in amlodipine besylate

A technology of amlodipine besylate and genotoxicity, which is applied in the field of drug analysis of methyl β-aminocrotonate, and can solve the problems of lack of detection methods for genotoxic impurities

Active Publication Date: 2020-11-17
BEIJING BAIAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In order to solve the problem of lack of genotoxic impurity detection method in the amlodipine besylate raw material medicine existing in the prior art, the present invention provides a kind of genotoxic impurity methyl β-aminocrotonate in amlodipine besylate Detection method

Method used

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  • Method for determining genotoxic impurities in amlodipine besylate
  • Method for determining genotoxic impurities in amlodipine besylate
  • Method for determining genotoxic impurities in amlodipine besylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Embodiment 1 method groping: methyl alcohol is diluent

[0045] (1) Instrument setting parameters

[0046] Direct injection method.

[0047] Chromatographic column: a capillary column with 6% cyanopropylphenyl-94% dimethylpolysiloxane as a stationary liquid (30m*0.53mm*3.0μm, OV-624 capillary column).

[0048] Heating program: the initial column temperature is 40°C, maintain for 5 minutes, increase the temperature to 220°C at 10°C / min, and maintain for 30 minutes;

[0049] Injection port: temperature is 220°C; column front pressure is 15kpa; column flow rate is 3.09ml / min; split ratio is 2:1;

[0050] The carrier gas is nitrogen;

[0051] Detector: hydrogen flame ionization detector (FID);

[0052] Carrier gas: nitrogen; detector temperature: 280°C.

[0053] Injection method: direct injection; the injection volume is 1 μl.

[0054] (2) Solution preparation

[0055] Standard stock solution: Take an appropriate amount of methyl β-aminocrotonate, accurately weigh it...

Embodiment 2

[0064] Embodiment 2 specificity and system applicability

[0065] (1) Preparation of solution

[0066] Standard stock solution: Take an appropriate amount of methyl β-aminocrotonate, accurately weigh it, and quantitatively dilute it with isopropanol to make a solution containing about 100 μg of methyl β-aminocrotonate per 1 ml, as a standard stock solution.

[0067] Standard reference substance solution: Accurately measure 2ml of standard stock solution, put it in a 20ml measuring bottle, dilute to the mark with isopropanol, shake well, and obtain the standard reference substance solution

[0068] Need testing solution: take about 200mg of this product, accurately weighed, add 2ml of isopropanol in precise amount, shake, filter, take the subsequent filtrate, as need testing solution (100mg / ml).

[0069] (2) Operation steps

[0070] Operation steps: Accurately measure 1.0 μl each of the blank solution (referring to isopropanol without methyl β-aminocrotonate), the standard re...

Embodiment 3

[0078] Embodiment 3 Sampling precision

[0079] (1) Preparation of solution

[0080] Same as Example 2

[0081] (2) Operation steps

[0082] Operation steps: Precisely measure 1.0 μl of the standard reference solution, inject it directly into the gas chromatograph, and record the chromatogram.

[0083] (3) Inspection results of injection precision

[0084] See the table below for the results of the injection precision inspection of methyl β-aminocrotonate.

[0085] Table 3: Methodology verification - inspection results of injection precision peak area

[0086] Methyl β-aminocrotonate 1 2 3 4 5 6 RSD(%) retention time (min) 17.124 17.125 17.125 17.127 17.128 17.126 0.01 Peak area 43.9 40.5 42.4 45.5 40.8 43.1 4.44

[0087] Conclusion: Using the direct sampling method, the reference substance solution was continuously injected 6 times, the RSD of the peak area of ​​β-aminocrotonate methyl ester was less than 10.0%, and the RSD v...

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Abstract

The invention provides a method for determining genotoxic impurities in amlodipine besylate. The method comprises the following steps: preparing a standard reference substance solution; preparing a test solution; precisely measuring the standard reference substance solution and the test sample solution, directly injecting into a gas chromatograph, recording a chromatogram, and calculating the amount of the beta-amino methyl crotonate in the test sample by peak area according to an external standard method. According to the method, the genotoxic impurity beta-amino methyl crotonate in the amlodipine besylate bulk drug is detected by adopting gas chromatography, so that the method has good precision and linearity, good durability for precolumn pressure, heating rate, column box initial temperature, sample inlet temperature and detection port temperature, high sensitivity and high sensitivity. The method is suitable for detecting the genotoxic impurity betaamino methyl crotonate in the amlodipine besylate bulk drug.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and in particular relates to a drug analysis method for determining a potential genotoxic impurity in amlodipine besylate: methyl β-aminocrotonate by using a GC method. Background technique [0002] Amlodipine besylate, chemical name: (±)-2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-1,4-dihydro-6-methyl -3,5-Pyridinedicarboxylate-5-methyl, 3-ethyl benzenesulfonate Molecular formula: C 20 h 25 ClN 2 o 5 ·C 6 h 6 o 3 S molecular weight: 567.06 Its structural formula is as follows: [0003] [0004] Amlodipine besylate belongs to dihydropyridine calcium ion antagonists, is a first-line long-acting antihypertensive drug, and is widely used clinically. Compared with other drugs, it has fewer contraindications and is very suitable for elderly hypertensive patients. In addition to lowering the blood pressure of patients, it also helps prevent the progression of atherosclerosis, prevent...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/68G01N30/86
CPCG01N30/02G01N30/06G01N30/68G01N30/8634G01N2030/047
Inventor 利虔刘延奎康彦龙孙志国张宪美方胜
Owner BEIJING BAIAO PHARMA
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