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HPLC with evaporative Light-scatter measuring method for huangyangning, cyclovirobuxine D, buxus alkaloid and relative alkaloid content

A high-performance liquid chromatography and Cyclovitamin technology, which is applied in the field of instrument analysis, can solve the problems of poor specificity of detection methods, and achieve the effect of strong specificity and appropriate sensitivity

Inactive Publication Date: 2007-09-26
杭太俊 +5
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to overcome the problem of poor specificity of existing detection methods, to provide a high-performance liquid chromatography evaporative light detection method for Buxus Ning, Cycloviral Buxus D, Buxus alkaloids and related alkaloids with suitable sensitivity and strong specificity. scatterometry

Method used

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  • HPLC with evaporative Light-scatter measuring method for huangyangning, cyclovirobuxine D, buxus alkaloid and relative alkaloid content
  • HPLC with evaporative Light-scatter measuring method for huangyangning, cyclovirobuxine D, buxus alkaloid and relative alkaloid content
  • HPLC with evaporative Light-scatter measuring method for huangyangning, cyclovirobuxine D, buxus alkaloid and relative alkaloid content

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The chromatographic column uses silica gel packing (Lichrospher SiO 2 , 4.6×250mm, 5μm).

[0041] 1. Determination of Cycloviral Buxicine D and Its Related Alkaloids

[0042] Chromatographic conditions and system adaptability: Silica gel is used as the filler for the stationary phase; tetrahydrofuran-methanol-acetonitrile-concentrated ammonia water (volume ratio 32:50:13:3) is used as the mobile phase; flow rate: 1mL min -1 ; Column temperature: 30°C; evaporative light scattering detector parameters: drift tube temperature 70°C, atomizing gas (N 2 ) flow rate: 1.5L min -1 ; In the chromatogram of the test solution, the peaks of Cycloviral Buxusine D and other alkaloid peaks should reach the baseline separation; the number of theoretical plates should be not less than 1000 based on the calculation of Cycloviral Buxusine D peak.

[0043] The configuration of the reference substance series solution (high concentration): take about 5, 6, and 8 mg of the reference substan...

Embodiment 2

[0056] Except that the mobile phase system was changed to ethyl acetate-methanol-concentrated ammonia water with a volume ratio of 15:3:2, and the flow rate of the mobile phase was 0.6mL min -1 , the column temperature is 25°C, the temperature of the drift tube in the evaporative light scattering detector is 65°C, and the nebulizing gas flow rate is 1.7L min -1 Outside, other is with embodiment 1. In the obtained chromatogram, the peak areas of its relevant alkaloids (peak numbers are 1, 2, 4, 5) are substituted into the low-concentration standard curve in turn, and the obtained contents are respectively 3.63%, 8.69%, 0.82%, and 0.91%. , the total content of the related alkaloids of cyclovir buxicine D is 14.05%.

Embodiment 3

[0058] Except that the mobile phase system was changed to ethyl acetate-acetonitrile-concentrated ammonia water with a volume ratio of 16:3:3.5, and the flow rate of the mobile phase was 1.6mL min -1 , the column temperature is 36°C, the temperature of the drift tube in the evaporative light scattering detector is 75°C, and the nebulizing gas flow rate is 1.3L min -1 Outside, other is with embodiment 1. In the obtained chromatogram, the peak areas of its relevant alkaloids (peak numbers are 1, 2, 4, 5) are substituted into the low-concentration standard curve in turn, and the obtained contents are respectively 3.60%, 8.63%, 0.83%, and 0.95%. , the total content of related alkaloids in Cyclovitamin D is 14.01%.

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Abstract

This invention discloses one high effective liquid phase spectrum evaporation diffusion test method for Huangyangning, ring Huangyangxing D and Huangyangsheng alkaloid and relative contents, which comprises the following steps: its color spectrum is fixed with silicon gel as stuff agent; the flow phase adopts tetrahydrofuran - carbinol - acetonitrile - intense ammonial solution or acetic acid ethyl ester - carbinol - intense ammonial solution; the test device adopts evaporation diffusion light tester.

Description

technical field [0001] The invention relates to an instrumental analysis method, in particular to a high performance liquid chromatography evaporative light scattering method for determining the contents of buxus ningen, cyclovir buxus D, buxus alkaloids and related alkaloids. Background technique [0002] Buxus mincrophylla Sieb.et Zucc.var.sinica Rehd.etWils., a plant of the family Buxus family, and the whole plant of the same genus, the total alkaloids obtained by extraction and conventional refining are called "Buxus Ning, Huowei Buxus D, or Buxus alkaloid", which belongs to the "effective part" of medicinal plants, and its main component "Cycloviric Buxus D" content is 60-80%; if it is separated and purified by high-performance liquid phase preparative column technology, its main component The content of "Cycloviral Buxus D" has risen to more than 90%, which can be renamed as "Cycloviral Buxus D", which belongs to the "active ingredient" of medicinal plants. [0003] T...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/60
Inventor 杭太俊张正行张梦翁静艳李丹袁厚亮
Owner 杭太俊
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