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Method for determining DCC content in indapamide bulk drug

A technology for indapamide and a determination method is applied in the field of determination of DCC content in indapamide raw materials, and achieves the effects of low toxicity, reliable and stable detection method, and less interference of impurities

Active Publication Date: 2020-05-19
GRAND PHARM (CHINA) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The liquid chromatography analysis method is a commonly used equipment for detection and analysis at present. It has many advantages such as rapidity, sensitivity, and good selectivity. Method for detecting DCC in dapamide bulk drug

Method used

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  • Method for determining DCC content in indapamide bulk drug
  • Method for determining DCC content in indapamide bulk drug
  • Method for determining DCC content in indapamide bulk drug

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] The analytical method verification results are as follows:

[0054] 1. System applicability:

[0055] Take the DCC reference substance solution and repeat the injection 6 times continuously, record the peak area of ​​the chromatogram, the results are as follows:

[0056] Table 1 Verification results of system adaptability

[0057]

[0058] 2. Specificity

[0059] Preparation of linear control stock solution: Accurately weigh 75mg of DCC, place in a 200ml measuring bottle, dissolve with ethanol and dilute to the mark, shake well, weigh 2ml of the solution into a 100ml measuring bottle, dilute to the mark with acetonitrile, and use as 100 % level reference substance solution.

[0060] Preparation of standard-added sample solution: Precisely weigh 125 mg of indapamide crude drug into a 25 ml measuring bottle, dissolve and dilute to the mark with the above-mentioned 100% level reference solution.

[0061] Get blank solvent (acetonitrile), DCC reference substance solu...

Embodiment 2

[0111] Get four different batches of indapamide crude drug and be mixed with need testing solution, respectively numbered 1-4, above-mentioned four kinds need testing solution and reference substance solution are carried out sampling detection according to above-mentioned chromatographic conditions respectively, wherein figure 1 Be numbered as the chromatogram of the need testing solution of 1, figure 2 Be numbered as the chromatogram of the need testing solution of 2, image 3 Be numbered as the chromatogram of the need testing solution of 3, Figure 4 Be numbered as the chromatogram of the need testing solution of 4, Figure 5 For the chromatogram of the DCC reference substance solution, the content of DCC in the need testing solution is calculated according to the external standard method by comparing with the DCC material peak area in the reference substance solution as shown in the table below:

[0112] Table 12 Content of DCC in different batches of indapamide raw mat...

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Abstract

The invention relates to a method for determining DCC content in an indapamide bulk drug. The method comprises the following steps: (1) preparing an indapamide bulk drug test solution; (2) preparing areference solution of DCC; (3) sample introduction: respectively detecting the test solution in the step (1) and the reference solution in the step (2) according to the following conditions: chromatographic conditions: a mobile phase: acetonitrile-water; gradient elution: gradually increasing the acetonitrile proportion from 44 to 46 percent to 94 to 96 percent in 0 to 20min, wherein the column temperature is 33-37 DEG C, and the flow rate is 1.4-1.6 ml / min and the detection wavelength is 190 -210 nm; and (4) calculating the peak area corresponding to DCC in the test sample and the referencesubstance solution to obtain the content of DCC. According to the method for determining the DCC content in the indapamide crude drug, the linear range is 1.506-15.060 mu g / ml, the detection limit is0.375 mu g / ml, and the recovery rate is greater than 95%. According to the method for determining the DCC content in the indapamide bulk drug, the used reagent is low in toxicity and impurity interference, the detection method is reliable and stable, and the method has important significance in quality control of the indapamide bulk drug.

Description

technical field [0001] The invention relates to a method for determining the content of DCC in indapamide crude drug. Background technique [0002] Indapamide is a sulfonamide diuretic with diuretic and calcium antagonistic effects. It is a strong and long-acting antihypertensive drug and is also clinically used for the treatment of water and sodium retention in congestive heart failure. DCC (dicyclohexylcarbodiimide) is a residue in the synthesis process of indapamide. The existence of DCC will affect the quality of the target product. Therefore, it is necessary to control this impurity to ensure that it does not exceed a certain limit range. At present, the national standard HG / T 5320-2018 only discloses the determination method of DCC mass fraction by gas chromatography. There is no detection method for DCC content in the prior art, let alone the DCC content in indapamide raw material medicine. However, the content of DCC in the bulk drug of indapamide is generally low, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/22G01N30/86
CPCG01N30/02G01N30/22G01N30/8679
Inventor 聂婷婷刘佩佩龚明峰蔡一聪陈小波余继梅
Owner GRAND PHARM (CHINA) CO LTD
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