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Method for separating and determining levocetirizine hydrochloride and genotoxic impurity E thereof by HPLC method

A technology for levocetirizine hydrochloride and genotoxicity, which is applied in the field of analytical chemistry to achieve the effects of strong specificity, good resolution and simple operation

Active Publication Date: 2020-04-10
CHONGQING HUABANGSHENGKAI PHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are currently no public reports on relevant detection methods

Method used

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  • Method for separating and determining levocetirizine hydrochloride and genotoxic impurity E thereof by HPLC method
  • Method for separating and determining levocetirizine hydrochloride and genotoxic impurity E thereof by HPLC method
  • Method for separating and determining levocetirizine hydrochloride and genotoxic impurity E thereof by HPLC method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] Mobile phase A: Weigh potassium dihydrogen phosphate 2.72 (0.02mol / L potassium dihydrogen phosphate) in a 1000ml volumetric flask, add water to dissolve and dilute to the mark, and adjust the pH value to 3.0±0.1 with phosphoric acid;

[0082] Mobile phase B: acetonitrile;

[0083] The volume ratio of mobile phase A and mobile phase B is 95:5.

[0084] (1) Preparation of solution

[0085] Preparation of impurity E solution: take about 25 mg of impurity E reference substance, put it in a 25ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well, and obtain impurity E stock solution.

[0086] Impurity E reference substance solution preparation: Precisely pipette 0.6ml of the above solution, put it in a 100ml measuring bottle, add diluent to dilute to the mark, and shake well to obtain a reference substance solution with an impurity E concentration of 6 μg / ml.

[0087] The preparation of levocetirizine hydrochloride need testing solution: take by w...

Embodiment 2 comparative example 1

[0094] Mobile phase A: water.

[0095] Mobile phase B: acetonitrile;

[0096] The volume ratio of mobile phase A and mobile phase B is 95:5.

[0097] Get the need testing solution prepared in embodiment 1 step 1) by above-mentioned chromatographic condition sampling, record chromatogram, measurement result is shown in Table 2.

[0098] Table 2 test results

[0099]

[0100] Conclusion: Different from mobile phase A in Example 1, the peak separation between impurity E and levocetirizine hydrochloride is 9.00, but the peak shape of impurity E is not good, not sharp, and the peak eluting time is late, so the sensitivity cannot meet the requirements. Adding salts to the mobile phase can advance the peak time and have a better peak shape.

Embodiment 3 comparative example 2

[0102] Mobile phase A: Weigh 0.92g of formic acid (0.02mol / L formic acid) into a 1000ml volumetric flask, add water to dissolve and dilute to the mark, and adjust the pH value to 3.0±0.1 with phosphoric acid;

[0103] Mobile phase B: acetonitrile;

[0104] The volume ratio of mobile phase A and mobile phase B is 95:5.

[0105] Get the need testing solution prepared in embodiment 1 step (1) by above-mentioned chromatographic condition sampling, record chromatogram, measurement result is shown in Table 3.

[0106] Table 3 test results

[0107]

[0108] Conclusion: In the separation test with the same other conditions as in the above example, except that the mobile phase A is different, the peak of impurity E appears, and the peak of levocetirizine hydrochloride does not appear, but the peak shape of impurity E is not good, not sharp, and the sensitivity cannot be satisfied Require. It is better to add salts to the mobile phase as buffer salts than to add acids as buffer sa...

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Abstract

The invention belongs to the field of analytical chemistry, and particularly relates to a method for separating and determining levocetirizine hydrochloride and a genotoxic impurity E thereof by an HPLC method. A chromatographic column adopted in the method takes octadecyl bonded silica gel as a filler, a mixed mobile phase of potassium dihydrogen phosphate and methanol and / or acetonitrile is adopted for elution, and a product enters a detector for detection. The method is a reversed-phase high performance liquid chromatography method. Separation and detection of levocetirizine hydrochloride and genotoxic impurities E thereof can be realized at the same time; the method has excellent separation performance and durability, is simple, convenient and feasible, has good reproducibility, is efficient and rapid, can achieve very good effects on tailing factors and theoretical pedal numbers, can effectively determine the content of genotoxic impurities E in levocetirizine hydrochloride, and has strong specificity.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for separating and measuring levocetirizine hydrochloride and its genotoxic impurity E by HPLC. Background technique [0002] Levocetirizine Hydrochloride (Levocetirizine Hydrochloride), listed in February 2001, is a third-generation antihistamine and a single optical isomer of the second-generation antihistamine cetirizine (cetirizine TP -isomer), developed by UCB, is a selective histamine H1 receptor antagonist, has no obvious anticholinergic and anti-serotonin effects, and has a small central inhibitory effect, and is mainly used for the treatment of respiratory system, skin and Allergic diseases of the eyes, such as allergic rhinoconjunctivitis, allergic skin diseases, allergic asthma, etc., have the advantages of quick onset of action, strong and long-lasting effect and few side effects. [0003] Levocetirizine hydrochloride is applicable to a wide r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/065
Inventor 林晓兵
Owner CHONGQING HUABANGSHENGKAI PHARM
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