Detection method for residual solvents of bilobalide B

A technology of ginkgolide and detection method, which is applied in the directions of measuring devices, instruments, scientific instruments, etc., can solve the problems of high instrument requirements, DMSO coagulation, inability to accurately sample and detect, etc., and achieve the effect of good separation effect and great application value.

Inactive Publication Date: 2015-12-23
SHANGHAI SINE PROMOD PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Provided 13 kinds of residual solvents for the detection of synthetic raw material fluoropaclitaxel, but this method uses dimethyl sulfoxide (DMSO) as the solvent, and the sampling method is headspace sampling, which has high requirements on the instrument. Moreover, although DMSO can Dissolve the sample, but when the temperature is low, DMSO solidifies, which cannot be accurately sampled and tested, which limits its application
At present, there is no report on the method for simultaneous detection of methanol, ethanol and ethyl acetate residues in ginkgolide B products, so further research design is needed

Method used

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  • Detection method for residual solvents of bilobalide B
  • Detection method for residual solvents of bilobalide B
  • Detection method for residual solvents of bilobalide B

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1 Sample detection and detection method repeatability experiment

[0021] Preparation of Ginkgolide B:

[0022] Take commercially available Ginkgo biloba extract extract (content standard is total lactone content ≥ 6%, total flavonoid content ≥ 24%, ginkgolic acid content ≤ 10ppm) 1000g, dilute to 0.5g crude drug / mL with 2000mL water, add 1000ml ethyl acetate Ethyl acetate was extracted three times in total, the ethyl acetate extract was combined, concentrated under reduced pressure at 45°C to no solvent, 100ml of 10% ethanol was added to make the concentration of the concentrated solution about 0.5g / mL, and the column was wet-packed to allow the liquid to pass through For MCI resin, first use 30% ethanol to elute the resin to remove impurities, to remove water-soluble and large polar impurities, elute 3BV in total, and the elution speed is 1BV / h, then use 40% ethanol to elute the resin at the same flow rate, after collection 3BV eluate, concentrated under redu...

Embodiment 2

[0033] Embodiment 2 Ginkgolide B sample detection

[0034]The preparation of ginkgolide B: get commercially available ginkgo biloba extract extract (content standard is total lactone content ≥ 6%, total flavonoid content ≥ 24%, ginkgolic acid content ≤ 10ppm) 1000g, dilute to 0.5g crude drug with aqueous solution / mL, add 1000ml ethyl acetate for extraction, extract three times in total, combine the ethyl acetate extracts, concentrate under reduced pressure at 45°C until there is no solvent, add 10% ethanol 100ml to make the concentration of the concentrated solution 0.5g / mL, and wet pack Column, let the drug solution pass through the MCI resin, first use 30% ethanol to elute the resin to remove impurities, to remove water-soluble and large polar impurities, a total of 3BV is eluted, and the elution speed is 1BV / h, and then 40% ethanol is used at the same flow rate Elute the resin, collect the 3BV eluate, concentrate it under reduced pressure at 45°C to 1g / ml extract, add 500m...

Embodiment 3

[0042] Embodiment 3 Ginkgolide B sample detection

[0043] The preparation of ginkgolide B: get commercially available ginkgo biloba extract extract (content standard is total lactone content ≥ 6%, total flavonoid content ≥ 24%, ginkgolic acid content ≤ 10ppm) 1000g, dilute to 0.5g crude drug with aqueous solution / mL, add 1000ml ethyl acetate for extraction, extract three times in total, combine the ethyl acetate extracts, concentrate under reduced pressure at 45°C until there is no solvent, add 10% ethanol 100ml to make the concentration of the concentrated solution 0.5g / mL, and wet pack Column, make the liquid medicine pass through the MCI resin, first elute the resin with 35% ethanol to remove water-soluble and polar impurities, and elute 3BV in total, the elution speed is 1BV / h, and then use 40% ethanol at the same flow rate Elute the resin, collect the 3BV eluate, concentrate it under reduced pressure at 45°C to 1g / ml extract, add 500ml of 80% methanol, heat to dissolve,...

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Abstract

The invention discloses a detection method for residual solvents of bilobalide B. The detection method comprises the following steps: (1) conducting a chromatographic condition and system suitability test; (2) preparing a control solution; (3) preparing a test solution; (4) measuring: respectively precisely sucking up a right amount of control solution and test solution, and directly injecting a sample into a gas chromatograph, measuring, calculating the content of methyl alcohol, ethyl alcohol and ethyl acetate by an external standard method, and finally, working out residual quantities of all the solvents in the bilobalide B. Proved by methodology validation, the detection method disclosed by the invention has a good separating effect, and limit of detection, limit of quantitation, linearity, stability, recovery rate and the like all meet the requirements; the detection method can be used for detecting the residual quantities of the methyl alcohol, the ethyl alcohol and the ethyl acetate in the ginkgolide B; the method is high in sensitivity and repeatability; by adopting a direct sample injection method, the method is simple in treatment, convenient in operation, suitable for industrial production and use, and has greater application value.

Description

technical field [0001] The invention relates to traditional Chinese medicines, in particular to a detection method for residual solvents in extracts of traditional Chinese medicines, in particular to a detection method for detection of ginkgolide B residual solvents. Background technique [0002] Ginkgo biloba is the leaf of Ginkgo biloba plant, the main chemical components are flavonoids and terpenoid lactones, which have important medicinal value and market value. Many Ginkgo biloba products have been developed in the market. With the progress of society and the development of economy, the importance of ginkgolides has attracted more and more attention. Among them, ginkgolide B, as a natural specific platelet activating factor (PAF) antagonist, has a certain effect on the treatment of stroke. Notable curative effect, its pharmacological action and therapeutic value have aroused great interest of the pharmaceutical industry. Ginkgolide B is obtained from Ginkgo biloba or G...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 胡林森孙蓉刘斐吕署一肖志勇李丁
Owner SHANGHAI SINE PROMOD PHARMA
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