CN1891242B

CN1891242B - Production process for removing polycyclic aromatic hydrocarbons from ginkgo leaf extract

Info

Publication number: CN1891242B
Application number: CN2005100804935A
Authority: CN
Inventors: 曹礼群; 李五洲; 蒋永红; 王建
Original assignee: JIYUAN NATURAL HEALTH PRODUCTS CO Ltd XUZHOU
Current assignee: Wuhu Luye Pharmaceutical Co Ltd
Priority date: 2005-07-06
Filing date: 2005-07-06
Publication date: 2012-01-04
Anticipated expiration: 2025-07-06
Also published as: CN1891242A

Abstract

The present invention relates to a process capable of utilizing organic solvent to make extraction and remove polycyclic aromatic hydrocarbon from the extract of ginkgo leaf. Said process mainly includes the following several steps: solvating, extraction and drying. As compared with existent technique, the polycyclic aromatic hydrocarbon content in the product can be effectively controlled so as to raise the quality of ginkgo leaf extract.

Description

A kind of production technology that from Folium Ginkgo extract, removes polycyclic aromatic hydrocarbon

Technical field

The present invention relates to a kind of production technology that removes the polycyclic aromatic hydrocarbon in the Folium Ginkgo extract.

Background technology

Polycyclic aromatic hydrocarbon (Polycyclic aromatic hydrocarbons is called for short PAHs) is meant the Hydrocarbon that contains two or more phenyl ring in the molecule, can be divided into aromatic condensed ring type and fragrant non-condensed ring type.The aromatic condensed ring type is meant that phenyl ring adjacent in the molecule has the Hydrocarbon of two shared carbon atoms at least, like naphthalene, anthracene, phenanthrene, pyrene etc.; The non-condensed ring type of fragrance is meant to have only the carbon atom chemical compound that links to each other between the phenyl ring adjacent in the molecule, like biphenyl, terphenyl etc.

Polycyclic aromatic hydrocarbon can cause canceration, and chemocarcinogenesis is meant that chemical substance causes that the process of tumor takes place to transform and develop into normal cell.Chemical carcinogen can be divided into directly acting carcinogens and indirect acting carcinogens, and polycyclic aromatic hydrocarbon belongs to the latter.Polycyclic aromatic hydrocarbon is to find the earliest and for one type of maximum chemical carcinogen of number, more than 2000 kinds of chemical compounds have been tested at present, finds to have the kind more than 500 that reaches of carcinogenesis, and wherein kind more than 200 is polycyclic aromatic hydrocarbon and derivant thereof.

Because polycyclic aromatic hydrocarbon and derivant thereof can cause canceration, countries in the world all begin biochemical article are formulated strict standard.Be defined in the air that the workman contacts 8h like U.S. Occupational Safety And Health office, coal tar and bituminous content must not surpass 0.2 μ g/m ³Germany requires benzo [a] pyrene content to be no more than 1 μ g/kg to the sootiness goods.China's drinking water standard regulation, benzo [a] pyrene must not surpass 0.01 μ g/L, and the waste water face is no more than 30 μ g/L, and the surface water is no more than 0.0025 μ g/L.And forbidding or restriction use regulations have also all been stipulated in each side various countries such as food, pesticide, cosmetics, discharge amount of exhaust gas.

Folium Ginkgo extract (EGB) is a kind of of many uses, natural materials of having no adverse reaction.Its effective ingredient mainly is ginkgetin and terpene lactone, has antagonism platelet activating factor (PAF), effects such as anti-cerebral ischemia anoxia, blood fat reducing, removing oxygen-derived free radicals, lax bronchial smooth muscle, antiallergic, antiinflammatory and enhancing nervous system activity.Clinical in EGB treatment treatment angina pectoris, cerebral ischemia, brain aging, alzheimer disease, brain insufficiency, asthma etc., received promising result.

Folium Ginkgo extract is used widely in medicine, health product, food service industry; But because environmental pollution; Cause in the Folium Ginkgo raw material in domestic many places of production and also contain polycyclic aromatic hydrocarbon; And China does not set up the limit standard of polycyclic aromatic hydrocarbon in the food at present, so the production method of present domestic Folium Ginkgo extract is not considered the residual quantity problem of polycyclic aromatic hydrocarbon, this certainly will influence the medicinal effects of Folium Ginkgo extract.Yet American-European countries has made strict regulation to the content of polycyclic aromatic hydrocarbon in the food, so, if do, will have influence on the outlet of Folium Ginkgo extract to European countries according to the production method of present domestic Folium Ginkgo extract.

In order to address the above problem, the present invention provides a kind of method that from Folium Ginkgo extract, removes polycyclic aromatic hydrocarbon, and this method is simple, and production cost is low, and removal efficiency is high, and the loss of effective components of Folium Ginkgo extract is smaller.

Summary of the invention

This patent goal of the invention is: remove the multiring aromatic hydrocarbon harmful components in the Folium Ginkgo extract, guarantee the product quality of Folium Ginkgo extract.

Technical problem to be solved by this invention is that a kind of production technology that removes the polycyclic aromatic hydrocarbon in the Folium Ginkgo extract is provided.

Technical scheme of the present invention is, extraction removes the polycyclic aromatic hydrocarbon in the Folium Ginkgo extract, and the step of its method is:

Ethanol or methanol in water heated and stirred are dissolved, cooling is placed, filtration with containing with Folium Ginkgo extract; Obtain Folium Ginkgo extract filtrating; Use organic extractant extraction Folium Ginkgo extract filtrating then, remove upper strata organic extraction phase, lower floor's aqueous solution of alcohol re-extract several times; Obtain through removing the Folium Ginkgo extract aqueous solution of alcohol of polycyclic aromatic hydrocarbon; Aqueous solution of alcohol is concentrated, dry then, obtain residual quantity summation＜20ppb (Folium Ginkgo extract product of benzopyrene＜5ppb) wherein of polycyclic aromatic hydrocarbon.Specifically: get Folium Ginkgo extract 10～100kg, adding concentration is 30～70% ethanol water or methanol aqueous solution 1000L, is heated to 40～60 ℃; Stirring and dissolving is placed cooled and filtered, obtains Folium Ginkgo extract and crosses cleaner liquid; Filtrating changes extractor over to, adds 500L cycloalkane then, standing demix behind the mix homogeneously; Remove upper strata cycloalkanes hydrocarbon phase, lower floor's aqueous solution of alcohol obtains passing through the Folium Ginkgo extract aqueous solution of alcohol that removes polycyclic aromatic hydrocarbon with fresh cyclohexane re-extract 5～9 times; Aqueous solution of alcohol is concentrated final drying.

Compare with prior art: product quality is except that indexs such as flavonoid of ginkgo biloba, bilobalide content, ginkgoic acid, heavy metal, microorganism are controlled; The residual of polycyclic aromatic hydrocarbon also is effectively controlled; Make that the use of Folium Ginkgo extract is safer and more effective, more help being exported to European Union member countries.

The specific embodiment

Come more detailed explanation the present invention below in conjunction with embodiment, but the present invention does not receive the restriction of these embodiment.

Embodiment 1:

Get Folium Ginkgo extract 10kg, adding concentration is 40～50% methanol aqueous solution 1000L, is heated to 40～50 ℃; Stirring and dissolving is placed cooled and filtered, obtains Folium Ginkgo extract and crosses cleaner liquid; Filtrating changes the 3000L extraction kettle over to, adds the 500L cyclohexane extraction then, standing demix behind the mix homogeneously; Remove upper strata cyclohexane extraction phase; The lower layer methanol aqueous solution obtains through removing the Folium Ginkgo extract aqueous solution of alcohol of polycyclic aromatic hydrocarbon with fresh cyclohexane re-extract 5 times, and it is residual with control methanol that the pure water that the Folium Ginkgo extract solution concentration that will contain methanol adds 100L to the 100L once more continues to be concentrated into 20～50L; Vacuum drying oven is dry, obtains removing the Folium Ginkgo extract of polycyclic aromatic hydrocarbon.

Measure the result: the PAHs total amount is 82.5ppb before removing, benzopyrene 3.1ppb, and removing back PAHs total amount is 15.8ppb, benzopyrene 0.8ppb.

Embodiment 2:

Get Folium Ginkgo extract 80～100kg, adding concentration is 40～50% ethanol water 1000L, is heated to 40～60 ℃; Stirring and dissolving is placed cooled and filtered, obtains Folium Ginkgo extract and crosses cleaner liquid; Filtrating changes the 3000L extraction kettle over to, adds the 500L cyclohexane extraction then, standing demix behind the mix homogeneously; Remove upper strata cyclohexane extraction phase, lower floor's ethanol water obtains passing through the Folium Ginkgo extract aqueous solution of alcohol that removes polycyclic aromatic hydrocarbon with fresh cyclohexane re-extract 7 times; Aqueous solution of alcohol is concentrated, and spray drying obtains removing the Folium Ginkgo extract of polycyclic aromatic hydrocarbon.

Measure the result: the PAHs total amount is 82.5ppb before removing, benzopyrene 3.1ppb, and removing back PAHs total amount is 11.7ppb, benzopyrene 0.7ppb.

The concrete content of embodiment 1 and 2 polycyclic aromatic hydrocarbon (PAHs) is as shown in table 1 below:

Table 1: the concrete content before and after polycyclic aromatic hydrocarbon (PAHs) removes

Sequence number	Chemical name	English name	Remove preceding PAHs (ppb)	Embodiment 1 PAHs (ppb)	Embodiment 2 PAHs (ppb)
						1	Naphthalene	Naphthalene	15.0	3.1	2.6
2	1, the inferior acenaphthene of 2-	Acenaphthylene	1.6	0.4	0.5
						3	Acenaphthene	Acenapthene	2.1	0.8	0.6
4	Fluorenes	Fluorene	0.9	0.7	0.4
						5	Luxuriant and rich with fragrance	Phenanthrene	7.9	1.6	1.2
6	Anthracene	Anthracene	2.6	0.7	0.6
						7	Fluoranthene	Fluoranthene	11.0	1.3	0.9
8	Pyrene	Pyrene	12.0	1.5	1.1
						9	Benzo [a] anthracene	Benzo(a)anthracene	5.0	0.7	0.6
10		Chrysene	8.4	1.6	1.0
						11	Benzo [b] fluoranthene	Benzo(b)fluoranthene	5.1	0.6	0.7
12	Benzo [k] fluoranthene	Benzo(k)fluoranthene	4.3	0.9	0.4
						13	Benzo [e] pyrene	Benzo(e)pyrene	3.1	0.8	0.7
14	Indeno [1,2,3] pyrene	Indeno(1，2，3)pyrene	1.8	0.7	0.4
						15	Dibenzanthracene	Dibenzoanthracene	1.0	0.2	0
16	Benzo [g, h, i] perylene	Benzo(g，h，i)perylene	0.7	0.2	0
						Add up to			82.5	15.8	11.7

Claims

1. production technology that from Folium Ginkgo extract, removes polycyclic aromatic hydrocarbon is characterized in that: get Folium Ginkgo extract 10～100kg, add concentration and be 30～70% ethanol water or methanol aqueous solution 1000L; Be heated to 40～60 ℃, stirring and dissolving is placed cooled and filtered; Obtain Folium Ginkgo extract and cross cleaner liquid, filtrating changes extractor over to, adds 500L cycloalkane then; Standing demix behind the mix homogeneously is removed upper strata cycloalkanes hydrocarbon phase, and lower floor's aqueous solution of alcohol is with fresh cyclohexane re-extract 5～9 times; Obtain through removing the Folium Ginkgo extract aqueous solution of alcohol of polycyclic aromatic hydrocarbon; Aqueous solution of alcohol is concentrated, and final drying obtains removing the Folium Ginkgo extract of polycyclic aromatic hydrocarbon.

2. the production technology that from Folium Ginkgo extract, removes polycyclic aromatic hydrocarbon according to claim 1 is characterized in that described cycloalkane is cyclohexane extraction.

3. the production technology that from Folium Ginkgo extract, removes polycyclic aromatic hydrocarbon according to claim 1, the residual quantity summation of polycyclic aromatic hydrocarbon that it is characterized in that Folium Ginkgo extract is less than 20ppb.

4. the production technology that from Folium Ginkgo extract, removes polycyclic aromatic hydrocarbon according to claim 1, the residual quantity that it is characterized in that the benzopyrene in the polycyclic aromatic hydrocarbon of Folium Ginkgo extract is less than 5ppb.