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Method for detecting levetiracetam enantiomer in levetiracetam raw material or sodium chloride injection

A technology of sodium chloride injection and enantiomers, which is applied in the field of detection of levetiracetam enantiomers, and can solve the problem of large polarity differences and symmetrical peak shapes of levetiracetam isomers Poor performance, undetectable and other problems, to achieve the effect of high accuracy

Active Publication Date: 2021-02-26
YANGTZE RIVER PHARM GRP NANJING HAILING PHARM CO LTD +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But pharmacopoeias such as European Pharmacopoeia and United States Pharmacopoeia only have the detection method of levetiracetam enantiomer, but there is no detection method of levetiracetam enantiomer in levetiracetam sodium chloride injection
[0004] Since levetiracetam sodium chloride injection is an aqueous solution, and the mobile phase for detecting levetiracetam enantiomers in the European Pharmacopoeia standard is a mixed solution of isopropanol and n-hexane, levetiracetam chloride Sodium injection can't dissolve with the flow in the European Pharmacopoeia standard, stratification occurs when the test solution is prepared, therefore, it is impossible to use the European Pharmacopoeia standard to detect levetiracetam in the levetiracetam sodium chloride injection. enantiomer
In the United States Pharmacopoeia standard, the mobile phase is a mixed solution of n-hexane and absolute ethanol, although the United States Pharmacopoeia standard mobile phase and levetiracetam sodium chloride injection are miscible, but because the United States Pharmacopoeia standard mobile phase and levetiracetam The polarity difference of racetam sodium chloride injection is large, and solvent effect will still occur, resulting in poor peak shape symmetry and low sensitivity of levetiracetam isomers; in addition, the AD-H chiral column used in the USP standard does not Suitable for the analysis of chiral systems, easy to damage the life of the chromatographic column

Method used

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  • Method for detecting levetiracetam enantiomer in levetiracetam raw material or sodium chloride injection
  • Method for detecting levetiracetam enantiomer in levetiracetam raw material or sodium chloride injection
  • Method for detecting levetiracetam enantiomer in levetiracetam raw material or sodium chloride injection

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Embodiment 1: System suitability experiment

[0058] Instrument: Agilent1260 high performance liquid chromatography; Chromatographic column: CHIRALPAK AGP (150mm×4mm, 5μm).

[0059] Chemical reagents: ammonia water (AR, Nanjing Chemical Laboratory); potassium dihydrogen phosphate (AR, Nanjing Chemical Laboratory); water (ultrapure water, self-made).

[0060] Sample to be tested: levetiracetam sodium chloride injection (manufacturer: Yangzijiang Pharmaceutical Group Nanjing Hailing Pharmaceutical Co., Ltd., batch number 18032221).

[0061] Reference substance: levetiracetam (content: 100%, manufacturer: European Pharmacopoeia, batch number: 3.0); levetiracetam enantiomer (content: 100%, manufacturer: European Pharmacopoeia, batch number: 3.0); Levetiracetam racemate (content: 100%, manufacturer: European Pharmacopoeia, batch number: R028T0).

[0062] System suitability solution: Dissolve the levetiracetam racemate reference substance in water to make a system suitabili...

Embodiment 2

[0073] Embodiment 2: specificity experiment

[0074] (1) Selectivity and interference test

[0075] Blank solution: water.

[0076] Blank auxiliary material solution: Take 1 mL of blank auxiliary material (take 8.2 g of sodium chloride, 1.64 g of sodium acetate, add water to dissolve and dilute to 1000 mL, adjust the pH to 5.5 with glacial acetic acid), put it in a 10 mL measuring bottle, add water to dilute to the mark, shake well, Instantly.

[0077] System suitability solution: Weigh the levetiracetam racemate reference substance and dissolve it in water to form a system suitability solution, wherein the concentrations of levetiracetam and levetiracetam enantiomers are both 0.05 mg / mL.

[0078] Levetiracetam enantiomer reference solution: Take about 4 mg of levetiracetam R isomer reference substance, weigh it accurately, add water to dissolve and dilute to 100 mL, shake well, and use as levetiracetam R Isomer reference stock solution. Precisely measure 1 mL of levetira...

Embodiment 3

[0090] Embodiment 3: Stability experiment

[0091] Prepare need testing solution and levetiracetam enantiomer reference substance solution according to embodiment 2, then need testing solution and levetiracetam enantiomer reference substance solution at room temperature, Place 48h, during this placement, need testing solution and levetiracetam enantiomer reference substance solution are carried out high-performance liquid chromatography detection respectively, detection condition is the same as embodiment 1, and detection result is as shown in table 3 :

[0092] Table 3 Stability Test

[0093]

[0094] It can be seen from Table 3 that the test solution and the levetiracetam enantiomer reference solution are still stable at room temperature for 48 hours.

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Abstract

The invention provides a method for detecting a levetiracetam enantiomer in a levetiracetam raw material or a sodium chloride injection, and belongs to the field of medicine quality detection. The detection method provided by the invention comprises the steps of diluting a levetiracetam raw material or a sodium chloride injection to obtain a test solution; and detecting the levetiracetam enantiomer in the test solution by adopting a high performance liquid chromatography, and calculating the content of the levetiracetam enantiomer in the levetiracetam sodium chloride injection according to a concentration-peak area standard curve of the levetiracetam enantiomer, wherein a chromatographic column of the high performance liquid chromatography is a chiral reversed phase chromatographic column,and the mobile phase is a phosphate buffer solution, and the pH value of the mobile phase is 5.0-6.0. The detection method provided by the invention can be used for detecting the content of the levetiracetam enantiomer in the levetiracetam sodium chloride injection, and is relatively high in accuracy.

Description

technical field [0001] The invention belongs to the field of drug quality detection, in particular to a method for detecting levetiracetam enantiomers in levetiracetam raw materials or sodium chloride injection. Background technique [0002] Levetiracetam (LEV) is a pyrrolidone derivative. In November 2011, the FDA approved the marketing of levetiracetam sodium chloride injection. When oral levetiracetam is ineffective, levetiracetam sodium chloride injection is used as an alternative treatment for adults (≥16 years old) with epilepsy. Levetiracetam can be used as an adjuvant treatment for partial seizures, adult myoclonic seizures and primary generalized tonic-clonic seizures in adults with epilepsy. It has broad-spectrum and rapid onset antiepileptic activity. Ideal pharmacokinetic properties, good tolerance and safety. However, its enantiomer (dexvetiracetam) has no pharmacological effect and is a degradation impurity, and its quality control must be carried out in the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/89G01N30/34
CPCG01N30/89G01N30/34
Inventor 刘仙仙孙净吴帆束晓峰李奉杰
Owner YANGTZE RIVER PHARM GRP NANJING HAILING PHARM CO LTD
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