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Method for detecting enantiomer content in levocarnitine

An enantiomer and content technology, applied in the field of drug detection, can solve the problem of high cost of derivatization reagents, and achieve the effects of low cost, high repeatability and accurate detection results.

Active Publication Date: 2017-06-13
SHANDONG QIDU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Levocarnitine recorded in the European Pharmacopoeia and the United States Pharmacopoeia does not control its enantiomer at present, in literature (J.Pharm.Biomed.Anal.30 (2002) 209-218), CN101723843A and CN102359995A etc. In the literature, after the derivatization of levocarnitine has been reported, the method for determining isomers by HPLC is reported, but the cost of derivatization reagents used in these methods is relatively high, so it is necessary to test the method for the content of enantiomers in levocarnitine. conduct more in-depth research

Method used

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  • Method for detecting enantiomer content in levocarnitine
  • Method for detecting enantiomer content in levocarnitine
  • Method for detecting enantiomer content in levocarnitine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Detection method:

[0046] 1. Chromatographic conditions:

[0047] Chromatographic column: CHIRAL IE chiral column, 250×4.6mm, particle size 5μm; detection wavelength 232nm; mobile phase: n-hexane-absolute ethanol-trifluoroacetic acid (volume ratio 70:30:0.3); column temperature: 30℃ ; Flow rate: 1.0ml / min; Running time: 25min; Injection volume: 10μl;

[0048] Blank solution: Derivative solution without levocarnitine.

[0049] 2. Solution configuration

[0050] 2.1 Configuration of dex-carnitine derivative stock solution:

[0051] Precisely weigh 10 mg of dex-carnitine derivative, put it in a 10ml volumetric flask, dissolve it with absolute ethanol to the mark, shake well, accurately measure 1ml, put it in a 20ml measuring bottle, add absolute ethanol to dilute to the mark, shake well, That is, the concentration is 0.05mg / ml;

[0052] 2.2 Configuration of system adaptability solution:

[0053] Accurately weigh 20mg of levocarnitine derivatives, put it in a 20ml vo...

Embodiment 2

[0061] Using benzoyl chloride as a derivatization reagent to detect the content of enantiomers in levocarnitine:

[0062] 1. Derivatization reaction of L-carnitine

[0063]Weigh 161mg of levocarnitine, put it in a reaction bottle, add 1.6ml of acetic acid and 168mg (1.2 equivalents) of benzoyl chloride, stir at 60-65°C for 0.5 hours, evaporate to dryness under reduced pressure, and obtain levocarnitine benzoyl chloride derivative things.

[0064] 2. Derivatization reaction of dex-carnitine

[0065] Weigh 161 mg of dex-carnitine, put it in a reaction bottle, add 1.6 ml of acetic acid and 168 mg (1.2 equivalents) of benzoyl chloride, stir at 60-65 ° C for 0.5 hours, evaporate to dryness under reduced pressure, and obtain dex-carnitine benzoyl chloride thing.

[0066] 3. Detect according to the detection method in Example 1, and the system suitability test results are shown in Table 1:

[0067] Table 1 System suitability test results

[0068]

[0069] See atlas Figures ...

Embodiment 3

[0076] Using p-ethylbenzoyl chloride as a derivatization reagent to detect the content of enantiomers in levocarnitine:

[0077] 1. Derivatization reaction of L-carnitine

[0078] Weigh 200mg of levocarnitine, put it in a reaction bottle, add 1.0ml of trifluoroacetic acid and 312mg (1.5 equivalents) of p-ethylbenzoyl chloride, stir at 65-70°C for 0.5 hours, and evaporate to dryness under reduced pressure to obtain levocarnitine Ting p-ethylbenzoyl chloride derivatives.

[0079] 2. Derivatization reaction of dex-carnitine

[0080] Weigh 200mg of dexcarnitine, put it in a reaction bottle, add 1.0ml of trifluoroacetic acid and 312mg (1.5 equivalent) of p-ethylbenzoyl chloride, stir at 65-70°C for 0.5 hours, evaporate to dryness under reduced pressure, and obtain dexcarnitine Ting p-ethylbenzoyl chloride derivatives.

[0081] 3. Detect according to the detection method in Example 1, the enantiomer content in the levocarnitine sample is 0.025wt%, the results are shown in Table 4...

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Abstract

The invention belongs to the technical field of medicine detection, and particularly relates to a method for detecting the content of an enantiomer in levocarnitine. According to the method, a benzoyl halide series compound is used as a derivatization reagent for derivatizing levocarnitine, high performance liquid chromatography (HPLC) is adopted for detection, and the content of the anantiomer is calculated through an area normalization method. The method for detecting the content of the enantiomer in levocarnitine is high in repeatability, precision and accuracy and is of great significance in controlling quality of levocarnitine active pharmaceutical ingredients and ensuring medication safety. In addition, the benzoyl halide series compound is used as the derivatization reagent, cost is low, a TLC method for monitoring the derivatization process displays that the derivatization reaction is complete, levocarnitine and the enantiomer thereof are completely converted into corresponding derivatives, and therefore accuracy of detection results is ensured.

Description

technical field [0001] The invention belongs to the technical field of drug detection, and in particular relates to a method for detecting the content of enantiomers in levocarnitine. Background technique [0002] Levocarnitine, also known as L-carnitine, is a component of food and widely exists in nature. The content in goat meat is the highest, about 2.1g / kg, while the content in plant food is very little or even none. Nutrients considered to be vitamin-like. The human body itself can also synthesize L-carnitine. There are about 20 grams of L-carnitine in the adult body, which is mainly distributed in the cardiac muscle and skeletal muscle. [0003] L-carnitine was first discovered in 1905 by Russian scientists Gulewitsch and Krimberg from muscle extracts. After years of research and development, L-carnitine has been widely used clinically. Its main function is to promote lipid metabolism. It can not only bring long-chain fatty acids into the mitochondrial matrix, promo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 任继波张涛高莹齐麟王水莲
Owner SHANDONG QIDU PHARMA
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