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Method for high performance liquid chromatography splitting of chiral drug lamivudine

A technology of high performance liquid chromatography and chiral drugs, which is applied in the field of separation of chiral drug lamivudine, can solve the problems of toxicity, low efficiency and ineffectiveness, and achieve wide application range, improved efficiency and accuracy, and good rigidity and thermal stability effects

Active Publication Date: 2016-09-28
广东顺德中科优联医学检验有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, it is found that a large part of the synthesized drugs have chirality, and one enantiomer in the chiral drug may be an active ingredient, which can match the chiral environment of the human body, so as to exert its due drug effect; while the other enantiomer body may be ineffective or even toxic

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  • Method for high performance liquid chromatography splitting of chiral drug lamivudine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1. Setting of chromatographic conditions

[0033] (1) The pH of the buffer solution triethylamine phosphate is 3.6, the volume ratio of the buffer solution triethylamine phosphate: organic modifier methanol and tetrahydrofuran mixture in the mobile phase is 40%: 60%, and degassing treatment is carried out by ultrasonic wave for 5 minutes.

[0034] (2) The detection temperature is 22°C.

[0035] (3) The flow rate of the mobile phase was set to 0.5 mL / min.

[0036] (4) The ultraviolet detection wavelength is set to 260nm.

[0037] 2. Injection for splitting

[0038] Run the high performance liquid chromatography column according to the above chromatographic conditions. When the baseline is stable and the baseline fluctuation is within 0.2mAu, use a micro injector to take 20 μL of the processed chiral drug lamivudine and inject it into the high performance liquid chromatography. In the sample injection system, split.

Embodiment 2

[0040] 1. Setting of chromatographic conditions

[0041] (1) The pH of the buffer solution triethylamine phosphate is 4.2, the volume ratio of the buffer solution triethylamine phosphate: organic modifier methanol and tetrahydrofuran mixture in the mobile phase is 45%: 55%, and degassing treatment is carried out by ultrasonic wave for 7 minutes.

[0042] (2) The detection temperature is 23°C.

[0043] (3) The flow rate of the mobile phase was set to 0.7 mL / min.

[0044] (4) The ultraviolet detection wavelength is set to 270nm.

[0045] 2. Injection for splitting

[0046] Run the high performance liquid chromatography column according to the above chromatographic conditions. When the baseline is stable and the baseline fluctuation is within 0.2mAu, use a micro injector to take 20 μL of the processed chiral drug lamivudine and inject it into the high performance liquid chromatography. In the sample injection system, split.

Embodiment 3

[0048] 1. Setting of chromatographic conditions

[0049] (1) The pH of the buffer solution triethylamine phosphate is 4.8, the volume ratio of the buffer solution triethylamine phosphate:organic modifier methanol and tetrahydrofuran mixture in the mobile phase is 50%:50%, and degassing treatment is carried out by ultrasonic wave for 10min.

[0050] (2) The detection temperature is 25°C.

[0051] (3) The flow rate of the mobile phase was set to 1.0 mL / min.

[0052] (4) The ultraviolet detection wavelength is set to 275nm.

[0053] 2. Injection for splitting

[0054] Run the high performance liquid chromatography column according to the above chromatographic conditions. When the baseline is stable and the baseline fluctuation is within 0.2mAu, use a micro injector to take 20 μL of the processed chiral drug lamivudine and inject it into the high performance liquid chromatography. In the sample injection system, split.

[0055] Under the chromatographic conditions set in the abo...

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Abstract

The invention discloses a method for high performance liquid chromatography splitting of a chiral drug lamivudine; a cyclodextrin type chiral column is used as a stationary phase, a buffer solution triethylammonium phosphate and an organic modifier are used as a mobile phase, a positive mobile phase system is adopted, and under conditions of the set temperature, flow velocity and UV detection wavelength, the chiral drug lamivudine is splitted; the organic modifier is a mixed solution of methanol and tetrahydrofuran which are mixed with the volume ratio of 9:1, and the organic modifier is subjected to suction filtration with a 0.22 [mu]m organic filter membrane before being used and is subjected to degassing treatment for 5-10 min by ultrasonic waves. The method has the advantages of high automation degree, simple operation, low cost and high efficiency, and has important practical guiding significance for research and use of lamivudine in medicines.

Description

【Technical field】 [0001] The invention relates to the technical field of biomedicine, in particular to a resolution method for chiral drug lamivudine. 【Background technique】 [0002] Chiral drugs refer to the introduction of a chiral center into the molecular structure of a drug, resulting in a pair of enantiomers that are the real object and the mirror image of each other. At present, it is found that a large part of the synthesized drugs have chirality, and one enantiomer in the chiral drug may be an active ingredient, which can match the chiral environment of the human body, so as to exert its due drug effect; while the other enantiomer The body may be ineffective or even toxic. Therefore, it is of great practical significance to develop and study the separation technology of chiral enantiomers for the quality control of medicine. [0003] Lamivudine is a pyrimidine nucleoside antiviral drug, mainly used for the treatment of chronic hepatitis B, it also has two isomers,...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027G01N2030/065
Inventor 滕钜海
Owner 广东顺德中科优联医学检验有限公司