Method for testing related substances of levocetirizine hydrochloride intermediate

A technology of levocetirizine hydrochloride and a determination method, applied in the field of analytical chemistry, can solve the problems of incomplete removal of impurities, influence on the purity and quality of drugs, etc., and achieve the effect of ensuring quality and controllable quality

Inactive Publication Date: 2015-04-29
AVENTIS PHARMA HAINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Impurities in the intermediate of levocetirizine hydrochloride are not completely removed, and will be introduced into the final product of the raw material drug, thereby affecting the purity and quality of the drug

Method used

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  • Method for testing related substances of levocetirizine hydrochloride intermediate
  • Method for testing related substances of levocetirizine hydrochloride intermediate
  • Method for testing related substances of levocetirizine hydrochloride intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Instruments and Conditions

[0037] High performance liquid chromatography: Shimadzu: LC-20AT, CBM-20A, SIL-20AC, SPD-M20A, CTO-10ASvp;

[0038] Column: C 18 (Kromasil, 250×4.6 mm, 5 μm);

[0039] Mobile phase: 0.02 mol / L potassium dihydrogen phosphate buffer solution (pH 3.0)-acetonitrile (60:40);

[0040] Flow rate: 1.0 mL / min

[0041] Detection wavelength: 230 nm

[0042] Column temperature: 25°C

[0043] Injection volume: 10 μL.

[0044] Experimental procedure

[0045] Take an appropriate amount of levocetirizine hydrochloride intermediate and its related substances, dissolve the samples in acetonitrile respectively, and prepare a sample solution containing about 0.5 mg / mL of levocetirizine hydrochloride intermediate and its related substances. Perform HPLC analysis according to the above conditions, and record the chromatograms. see attached results Figure 1~2 , figure 1 The chromatographic peak whose retention time is 12.529 min is the levocetirizine h...

Embodiment 2

[0047] Instruments and Conditions

[0048] High performance liquid chromatography: Shimadzu: LC-20AT, CBM-20A, SIL-20AC, SPD-M20A, CTO-10ASvp;

[0049] Column: C 18 (Kromasil, 250×4.6 mm, 5 μm);

[0050] Mobile phase: 0.02 mol / L sodium dihydrogen phosphate buffer solution (pH 3.0)-acetonitrile (65:35);

[0051] Flow rate: 1.0 mL / min

[0052] Detection wavelength: 230 nm

[0053] Column temperature: 25°C

[0054] Injection volume: 10 μL.

[0055] Experimental procedure

[0056] Take an appropriate amount of levocetirizine hydrochloride intermediate and its related substances, dissolve the samples in acetonitrile respectively, and prepare a sample solution containing about 0.5 mg / mL of levocetirizine hydrochloride intermediate and its related substances. Perform HPLC analysis according to the above conditions, and record the chromatograms. see attached results Figure 3~4 , image 3 The chromatographic peak whose retention time is 22.297 min is the levocetirizine hydro...

Embodiment 3

[0058] Instruments and Conditions

[0059] High performance liquid chromatography: Shimadzu: LC-20AT, CBM-20A, SIL-20AC, SPD-M20A, CTO-10ASvp;

[0060] Column: C 18 (Kromasil, 250×4.6 mm, 5 μm);

[0061] Mobile phase: 0.02 mol / L dipotassium hydrogen phosphate buffer solution (pH 6.0)-acetonitrile (65:35);

[0062] Flow rate: 1.0 mL / min

[0063] Detection wavelength: 230 nm

[0064] Column temperature: 25°C

[0065] Injection volume: 10 μL.

[0066] Experimental procedure

[0067] Take an appropriate amount of levocetirizine hydrochloride intermediate and its related substances, dissolve the samples with acetonitrile respectively, and prepare a sample solution containing about 0.5 mg / mL of levocetirizine hydrochloride intermediate and its related substances; another appropriate amount of acetonitrile is used as blank solvent. Perform HPLC analysis according to the above conditions, and record the chromatograms. see attached results Figure 5~7 , Figure 5 is the solven...

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Abstract

The invention belongs to the field of analytical chemistry, and discloses a method for separately testing a levocetirizine hydrochloride intermediate and related substances of the levocetirizine hydrochloride intermediate by liquid chromatography. The method comprises the following steps: a chromatographic column taking octadecylsilane chemically bonded silica as a filler uses a certain proportion of buffer salt solution-organic phase as a mobile phase to quantificationally test the content of the levocetirizine hydrochloride intermediate and the content of the related substances of levocetirizine hydrochloride intermediate, so that the quality of the levocetirizine hydrochloride intermediate is effectively controlled, and the controllable quality of levocetirizine hydrochloride is ensured. The method is high in specificity and accuracy, and simple and convenient to operate.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, in particular to a method for separating and measuring levocetirizine hydrochloride intermediates and related substances by liquid chromatography. Background technique [0002] Levocetirizine hydrochloride is used to relieve allergic symptoms of allergic diseases, clinically used to treat allergic rhinitis, urticaria, angioedema and other skin and mucous membrane allergic diseases, and also used to reduce allergic symptoms of colds . The chemical name of the intermediate of levocetirizine hydrochloride is 2-(4-((4-chlorophenyl)(phenyl)methyl)piperazin-1-yl)ethanol, and the molecular formula is C 19 h 23 ClN 2 O. The structural formula of levocetirizine hydrochloride intermediate is: [0003] . [0004] In the process of synthesizing this compound, some important intermediates may affect the purity and quality of the drug due to incomplete removal. For the synthesis of levocetirizine hy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 杨敏王宇杰马苏峰
Owner AVENTIS PHARMA HAINAN
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