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Method for separation and determination of metaraminol bitartrate and its isomers by high performance liquid chromatography

A technology of meta-hydroxylamine bitartrate and high performance liquid chromatography, which is applied in the field of analytical chemistry, can solve the problems such as no literature reports in the separation and determination of meta-hydroxylamine bitartrate and its isomers, and achieves the effect of ensuring effectiveness and safety

Active Publication Date: 2019-03-26
CHANGZHOU SUNLIGHT PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Although various methods are used to control the other three isomers in the preparation process of metaraminol bitartrate, there will still be a certain amount of isomers in the final metaraminol bitartrate bulk drug
[0010] The separation of optical isomers of compounds containing multiple chiral carbon atoms has always been a difficult point in the quality control of chiral drugs. However, the separation and determination of metaraminol tartrate and its isomers has not been reported in the literature so far

Method used

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  • Method for separation and determination of metaraminol bitartrate and its isomers by high performance liquid chromatography
  • Method for separation and determination of metaraminol bitartrate and its isomers by high performance liquid chromatography
  • Method for separation and determination of metaraminol bitartrate and its isomers by high performance liquid chromatography

Examples

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experiment example )

[0032] This experimental example is a method for the separation and determination of metaraminol tartrate and its isomers by high performance liquid chromatography.

[0033] 1. Instruments.

[0034] High performance liquid chromatography: Shimadzu, LC-20A, SPD20-UV detector.

[0035] Chromatographic column: CHIRALPAK AD-H (4.6×250mm, 5μm).

[0036] 2. Chromatographic conditions.

[0037] Mobile phase: n-hexane: absolute ethanol: isopropylamine (80:20:0.2).

[0038] Flow rate 1.0 mL / min.

[0039] Detection wavelength: 220nm.

[0040] Column temperature: 30°C

[0041] Injection volume: 20 μL.

[0042] Three: Experimental steps.

[0043] Weigh 2.5 mg of metaraminol bitartrate and its three isomers respectively, place in a 10 mL measuring bottle, add ethanol to dissolve and dilute to the mark, shake well to obtain a system suitability solution.

[0044] Accurately measure 20 μL each of the blank solution and the above-mentioned system suitability solution, perform high-per...

Embodiment 1)

[0048] This embodiment is a method for the separation and determination of metaraminol bitartrate crude drug by high performance liquid chromatography.

[0049] 1. Instruments.

[0050] Same as the experimental example.

[0051] 2. Chromatographic conditions.

[0052] Same as the experimental example.

[0053] Three: Implementation steps.

[0054] Weigh 10 mg of metaraminol tartrate crude drug, place in a 10 mL measuring bottle, add ethanol to dissolve and dilute to the mark, shake well, as the test solution.

[0055] Precisely measure 20 μL of the test solution, carry out high-performance liquid chromatography analysis according to the above conditions, record the chromatogram, and see the results in image 3 .

[0056] image 3 The chromatographic peak whose retention time is 28.616min is the chromatographic peak of metaraminol tartrate.

[0057] Depend on image 3 It can be seen that the method of the present invention can effectively measure the content of enantiom...

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Abstract

The invention discloses a method for separating and detecting metaraminol bitartrate and isomers thereof through high performance liquid chromatography. The method adopts a chiral chromatographic column, and adopts an n-hexane, anhydrous ethanol and isopropylamine mixed solution as a mobile phase; a volume ratio of n-hexane to anhydrous ethanol to isopropylamine in the mobile phase is (60-95):(5-30):(0.05-0.5); and the chiral chromatographic column is a bonded chiral chromatographic column adopting silica gel with the surface covalently bonded with amylose-tris(3,5-dimethylphenylcarbamate) as a filler. Separation and detection of the metaraminol bitartrate and the isomers thereof are realized by adopting the high performance liquid chromatography and the chiral chromatographic column, especially creatively making the special mobile phase, so the effectiveness and the safety of the metaraminol bitartrate is finally guaranteed.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a method for separating and measuring metaraminol bitartrate and its isomers by high performance liquid chromatography. Background technique [0002] Metaraminol Bitartrate is the bitartrate of Metaraminol Bitartrate. It is an α-adrenoceptor agonist developed by Fresenius Kabi Company in the United States. It mainly acts on α-receptors. It is suitable for early treatment of shock and prevention of spinal Acute hypotension during internal block anesthesia. [0003] Due to the existence of two chiral carbon atoms in metaraminol tartrate, there are four configurations (1R, 2S), (1S, 2R), (1R, 2R), (1S, 2S), among which (1R, 2S) is the effective configuration, (1S, 2R) is its enantiomer, and (1R, 2R) and (1S, 2S) are its diastereomers. [0004] The four configuration structures of metaraminol are as follows: [0005] (1R, 2S) configuration: . [0006] (...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/34
CPCG01N30/02G01N30/34
Inventor 胡国宜胡锦平汪士金刘建辉姚丽娜曲丽娜奚小金
Owner CHANGZHOU SUNLIGHT PHARMA
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