Method for determination of residual solvents in ginkgo leaf extract by headspace gas chromatography

A headspace gas chromatography and residual solvent technology, which is used in measuring devices, instruments, scientific instruments, etc., to achieve the effect of simple and convenient sample processing, extended analysis time, and good separation.

Inactive Publication Date: 2018-01-19
SHANGHAI SINE PROMOD PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The main residual solvents in Ginkgo biloba extract products are cyclohexane, ethanol and ethyl acetate, and there is no report on the detection method of Ginkgo biloba extract organic solvent residues

Method used

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  • Method for determination of residual solvents in ginkgo leaf extract by headspace gas chromatography
  • Method for determination of residual solvents in ginkgo leaf extract by headspace gas chromatography
  • Method for determination of residual solvents in ginkgo leaf extract by headspace gas chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1 Sample detection and detection method repeatability experiment

[0023] Preparation of Ginkgo biloba extract:

[0024] Take 100kg of ginkgo leaves, add water-containing ethanol for reflux extraction twice, add 750L of 80% ethanol for reflux extraction for 2 hours for the first time, add 650L of 70% ethanol for 2 hours for reflux extraction for the second time, add 500L water for reflux extraction for 2 hours for the third time, Combine the first two ethanol extracts, concentrate under reduced pressure until there is no alcohol smell, add 200L of cold water, stir evenly, let stand overnight, filter with suction, collect the filtrate, combine with the water extract, pass through polyamide 35L D-101 resin, Wash 100L with water, collect and set aside, then elute 70L with 70% ethanol, concentrate under reduced pressure to 10L, extract 3 times with ethyl acetate, each extraction volume is 12L, 10L, 8L respectively, and collect the extract and raffinate respectively ...

Embodiment 2

[0033] Example 2 Ginkgo biloba extract sample detection

[0034] Preparation of Ginkgo biloba extract:

[0035]Take 100 kg of ginkgo leaves, add water-containing ethanol for reflux extraction twice, first add 800 L of 80% ethanol for reflux extraction for 2 hours, add 600 L of 70% ethanol for the second time for reflux extraction for 2 hours, and add 600 L of water for the third time for reflux extraction for 2 hours. Combine the first two ethanol extracts, concentrate under reduced pressure until there is no alcohol smell, add 150L of cold water, stir evenly, let stand overnight, filter with suction, collect the filtrate, combine with the water extract, pass through polyamide 35L D-101 resin, Wash 100L with water, collect and set aside, then elute 70L with 70% ethanol, concentrate under reduced pressure to 10L, extract 3 times with ethyl acetate, each extraction volume is 12L, 10L, 8L respectively, and collect the extract and raffinate respectively , the extract was concentr...

Embodiment 3

[0043] Example 3 Ginkgo biloba extract sample detection

[0044] Preparation of Ginkgo biloba extract:

[0045] Take 100kg of ginkgo leaves, add water-containing ethanol for reflux extraction twice, first add 600L of 80% ethanol for reflux extraction for 2 hours, add 700L of 70% ethanol for the second time for reflux extraction for 2 hours, and add 550L of water for the third time for reflux extraction for 2 hours, Combine the first two ethanol extracts, concentrate under reduced pressure until there is no alcohol smell, add 180L of cold water, stir evenly, let stand overnight, filter with suction, collect the filtrate, combine with the water extract, pass through polyamide 35L D-101 resin, Wash 100L with water, collect and set aside, then elute 70L with 70% ethanol, concentrate under reduced pressure to 10L, extract 3 times with ethyl acetate, each extraction volume is 12L, 10L, 8L respectively, and collect the extract and raffinate respectively , the extract was concentrate...

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Abstract

The invention relates to a method for determination of residual solvents in a ginkgo leaf extract bulk drug by headspace gas chromatography. The method includes the steps of: (1) chromatographic condition and system suitability test; (2) preparation of a reference solution and a test solution; and (3) determination: injecting the reference solution and the test solution respectively into a gas chromatograph by headspace sampling, and calculating the content of cyclohexane, ethanol and ethyl acetate by external standard method. Methodology validation indicates that the method provided by the invention has good separation degree, has detection limit, quantitation limit, linearity, stability, standard adding recovery rate and the like all meeting the requirements, and can be used for residualdetection of cyclohexane, ethanol and ethyl acetate in the ginkgo leaf extract. The analysis method for simple, fast and accurate detection of the ginkgo leaf extract solvent residue is suitable forindustrial production, and has great application value.

Description

technical field [0001] The invention relates to traditional Chinese medicines, in particular to a method for detecting residual solvents in traditional Chinese medicine extracts, in particular to a method for determining residual solvents in ginkgo leaf extracts by headspace gas chromatography. Background technique [0002] As the quality requirements for food and pharmaceuticals become more and more stringent, the requirements for residual solvent analysis and detection of products that use organic solvents in the production process are getting higher and higher. Ginkgo biloba extract is extracted from Ginkgo biloba and is used to treat blood stasis type chest pain (angina pectoris of coronary heart disease) and blood stasis type mild cerebral arteriosclerosis caused by dizziness. The main residual solvents in Ginkgo biloba extract products are cyclohexane, ethanol and ethyl acetate, and there is no report on the detection method of Ginkgo biloba extract organic solvent res...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 李丁孙蓉李玉杰刘斐
Owner SHANGHAI SINE PROMOD PHARMA
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