Method for measuring DD-captopril and LD-captopril in captopril bulk drug by using HPLC method

A raw material drug, topril technology, applied in the direction of measuring devices, material separation, analysis of materials, etc., can solve the problem of unchecked captopril isomers, DD-captopril and LD-captopril Research and other issues, to achieve the effect of strong specificity, good separation, and high precision

Inactive Publication Date: 2020-01-24
SHANDONG XINHUA PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] According to literature review, there is currently no report on the detection method of captopril isomers DD-captopril and LD-captopril, and there is no record in the national pharmacopoeia standards. The European Pharmacopoeia uses pre-column Derivatization-gas chromatography only determined the content of impurity F in captopril, but did not study DD-captopril and LD-captopril

Method used

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  • Method for measuring DD-captopril and LD-captopril in captopril bulk drug by using HPLC method
  • Method for measuring DD-captopril and LD-captopril in captopril bulk drug by using HPLC method
  • Method for measuring DD-captopril and LD-captopril in captopril bulk drug by using HPLC method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] The content determination of DD-captopril and LD captopril in embodiment 1 captopril crude drug

[0046] (1) Preparation of impurity reference substance stock solution

[0047] Mixed impurity reference substance stock solution: Accurately weigh about 5mg of DD-captopril and about 5mg of LD-captopril into the same 50mL measuring bottle, add absolute ethanol to dissolve and dilute to the mark, shake well, and obtain.

[0048] Single impurity reference substance stock solution: Accurately weigh about 2 mg each of DD-captopril, LD-captopril, impurity F, and captopril reference substance, place them in 20mL measuring bottles, add absolute ethanol to dissolve And dilute to the mark, shake well, that is.

[0049] (2) Preparation of system suitability solution

[0050] Accurately weigh about 50 mg of the captopril reference substance into a 10mL measuring bottle, add precisely pipetted 0.5mL mixed impurity reference substance stock solution, add absolute ethanol and dilute to...

Embodiment 2

[0072] Embodiment 2 changes mobile phase ratio

[0073] By fine-tuning the proportion of the mobile phase, it was investigated whether the method is still applicable when the proportion of the mobile phase changes slightly; other conditions are the same as in Example 1 except for a slight change in the proportion of the mobile phase.

[0074] Precisely measure 10 μL of the system suitability solution and inject it into the liquid chromatograph, and record the liquid chromatogram. The change of part of the mobile phase ratio leads to inconsistency among DD-captopril, LD-captopril, and captopril. Therefore, the method should strictly control the ratio of the mobile phase, but the three can be completely separated by fine-tuning the ratio of the mobile phase. The results are shown in Table 3 below.

[0075] Table 3 Example 2 system suitability result

[0076]

Embodiment 3

[0077] Embodiment 3 changes column temperature

[0078] Investigate whether the method is still applicable when the column temperature changes slightly; except that the column temperature is adjusted to 28°C and 32°C respectively, other conditions are the same as in Example 1.

[0079] Precisely measure 10 μL of the system suitability solution and inject it into the liquid chromatograph, record the liquid chromatogram, when the column temperature is adjusted to 28°C and 32°C, DD-captopril, LD-captopril, and captopril three The degree of separation between them is greater than 1.5, which can realize complete separation. The results are shown in Table 4 below.

[0080] Table 4 Embodiment 3 system suitability result

[0081]

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Abstract

The invention discloses a method for measuring DD-captopril and LD-captopril in a captopril bulk drug by using an HPLC method. A normal phase liquid chromatography is adopted, a chromatographic columnadopts an amylose-tri(5-chlorine-2-methylphenyl carbamate) coating filler, a mobile phase is n-hexane-isopropanol-ethanol- trifluoroacetic acid, the volume ratio of which is 85: 10: 5: 0.1, the detection wavelength is 215 nm, the flow rate is 0.95 to 1.05 mL / min, the column temperature is 28 to 32 DEG C, and the injection volume is 10 muL. A system applicability test is performed according to themethod provided by the invention, the captopril, DD-captopril and LD-captopril can be effectively separated, the method is high in specificity, good in resolution and high in precision, the signal-to-noise ratio of an own contrast solution is greater than 10, and the contents of the DD-captopril and LD-captopril in the captopril bulk drug can be quantitatively measured, thereby effectively controlling the quality of captopril raw materials.

Description

technical field [0001] The invention belongs to the technical field of drug analysis and relates to a method for measuring D-captopril and LD-captopril in captopril raw materials by high performance liquid chromatography (HPLC). Background technique [0002] Captopril is the earliest discovered angiotensin converting enzyme inhibitor (ACEI), which is widely used in various types of hypertension. , Rheumatoid arthritis, hyperthyroidism and other diseases clinical drug development, and achieved good clinical results. [0003] Captopril, also known as mercaptomethylpropaproline, has a structural formula such as figure 1 , there are two chiral centers in its structure, there are three stereoisomers, respectively LL-captopril, DD-captopril, LD-captopril, its structural formula is as Figure 2 ~ Figure 4 , In the European Pharmacopoeia Raw Material Standards, there are 15 impurities from captopril impurity A to impurity O, wherein impurity F is an isomer impurity, i.e. LL-captop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 尹延丽曹文冰徐涛
Owner SHANDONG XINHUA PHARMA CO LTD
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