CN108485817B

CN108485817B - Method for extracting herba Filipendulae extract

Info

Publication number: CN108485817B
Application number: CN201810588346.6A
Authority: CN
Inventors: 唐贵才; 姜永久; 贾清文; 徐文哲; 王同月
Original assignee: Baishan science and technology research institute
Current assignee: Baishan Heitu Agricultural Technology Co.,Ltd.
Priority date: 2018-06-08
Filing date: 2018-06-08
Publication date: 2021-07-23
Anticipated expiration: 2038-06-08
Also published as: CN108485817A

Abstract

A method for extracting a Filipendula vulgaris extract relates to the field of Filipendula vulgaris processing, and solves the problem of low extraction rate of the existing method for extracting the Filipendula vulgaris extract. The invention comprises the following steps: pretreating a Filipendula ulmaria raw material, leaching, concentrating under reduced pressure, recovering a solvent and obtaining a Filipendula ulmaria extract product. The invention mainly adopts a static and dynamic leaching and a flower bed fixed solvent circulation leaching extraction process to prepare the Filipendula repens extract, researches the extraction process of the Filipendula repens extract, researches the influence of the Filipendula repens extract on the extract yield in the aspects of the Filipendula repens harvesting time, the content determination of the extract at different parts, the leaching time, the leaching mode and the like, performs fragrance evaluation and application tests on the obtained product, and provides a scientific basis for guiding production. The invention has simple process and equipment, less investment, no waste of raw materials, low cost, good quality of the extract and high yield, and the yield of the extract can reach 0.48 percent.

Description

Method for extracting herba Filipendulae extract

Technical Field

The invention relates to the technical field of processing of Filipendula esculenta, and particularly relates to a method for extracting Filipendula esculenta extract.

Background

Filipendula officinalis is a perennial herb of the genus Filipendula of the family Rosaceae (Rosaceae), and is commonly grown in hillsides, riverside wetlands, meadows and forest edges. The height is 1-1.4 m. The rootstock is thick and strong, and the rootstock is horizontal and has more fibrous roots. Upright diameter, thick, thin edge, smooth, tan. Leaf intergrowth, pinnate compound leaf or discontinuous pinnate compound leaf; the basal leaves and the lower cauline leaves have long stems; the leaf quality is thick; the small leaves at the top end are extra large, the palm shape is 7-9 deep cracks, and the length is 8-13 cm. The width of the leaf is 12-15 cm, the split piece is in a shape of a wide needle or a long round needle, the tip of the leaf is gradually sharp or long and gradually sharp, and irregular and thick sawteeth are arranged at the edge of the leaf. The upper side is green, the lower side is dense white villi, and veins are convex; a pair of lobules are lateral, often with 3 cleft; big leaf, half heart, chamber-shaped, coniform, big; small and most flowers; calyx 4 is fissured; petals 5, white, round or nearly round, 3 mm long; stamens are numerous and longer than petals; 6-8 of carpel. The lean fruit has a handle, a half moon shape, and eyelashes, flower pillars and calyx at the edge for storing. The calyx is reversely broken, the flowering phase is 6-7 months, and the fruit phase is 7-9 months. Growing in hilly grassland, riverside wetlands, meadows and forest edges. Distributed in northeast, northeast China, Korea, northern Japan, Mongolia, Siberian Su-Union and the far east.

Since the mosquitos are fragrant and pleasant in flowering phase and form a strong and elegant fragrance which integrates the effects of freshness, freshness and sweetness, the mosquitos are widely used in spice processing.

At present, the extraction rate of the Filipendula ulmaria extract extracted by adopting the traditional solvent extraction method is about 0.35 percent, the extraction rate is lower, the raw materials are seriously wasted, and the cost is increased.

Disclosure of Invention

The invention provides a method for extracting a herba Filipendulae extract, aiming at solving the problem of low extraction rate of the existing method for extracting the herba Filipendulae extract.

The technical scheme adopted by the invention for solving the technical problem is as follows:

the invention relates to a method for extracting a Filipendula ulmaria extract, which comprises the following steps:

step one, raw material pretreatment

When 70% of flowers of the Filipendula esculenta are open in 6-7 months, harvesting the Filipendula esculenta raw material, and removing withered leaves and thick stalks on the lower part;

step two, putting the raw materials into flower columns, wherein the materials are required to be uniformly charged, weighing, wherein the upper flower column and the lower flower column are a tank, and 300-350 kg of materials are charged in each tank;

step three, putting the flower column into an extraction tank by using an electric hoist;

step four, injecting petroleum ether with a boiling range of 60-70 ℃ into the storage tank, wherein the material-liquid ratio is as follows: the raw material is petroleum ether which is 1: 3;

step five, statically soaking for 2.5 hours, then opening a valve of a circulating system, starting the circulating pump to circulate for 30 minutes, and then circulating once every 1 hour for six hours in total and circulating for three times;

step six, after leaching, pumping the leaching liquor into a concentration tank, washing residues twice by using petroleum ether, wherein the using amount of the petroleum ether in each time is the same, and the volume ratio is as follows: leaching liquor, namely petroleum ether, is 1:2.5, and the washing time is 30 minutes respectively;

seventhly, controlling the solvent in the residues in the leaching tank to be clean, closing a circulating system, opening a distillation system, introducing steam into the leaching tank for 30 minutes, and blowing out residual petroleum ether;

step eight, opening a steam switch of the falling film evaporator, and controlling a pressure gauge to be 0.1 Mpa;

step nine, opening a valve of a concentration tank for concentration, and condensing a solvent through a condenser to enter a storage tank for reuse;

step ten, controlling the concentration speed, completing the concentration within two hours, and concentrating to 3-5 liters of concentrated solution;

step eleven, filtering the concentrated solution, and carrying out reduced pressure concentration in a 3-5L flask until petroleum ether completely flows out;

step twelve, adding absolute ethyl alcohol, and continuing to concentrate until the solvent does not drip out;

thirteen, discharging, cooling to room temperature to obtain dark green paste;

and step fourteen, weighing, bottling and warehousing.

In a preferred embodiment, in the seventh step, the blown petroleum ether is cooled and then is fed into a reaction kettle for deodorization treatment, and the petroleum ether can be recycled after the treatment.

The invention has the beneficial effects that: the invention mainly adopts a static and dynamic leaching and a flower bed fixed solvent circulation leaching extraction process to prepare the Filipendula repens extract, researches the extraction process of the Filipendula repens extract, researches the influence of the Filipendula repens extract on the extract yield in the aspects of the Filipendula repens harvesting time, the content determination of the extract at different parts, the leaching time, the leaching mode and the like, performs fragrance evaluation and application tests on the obtained product, and provides a scientific basis for guiding production.

The mosquito-grass extract obtained by the invention is evaluated for fragrance by experts in the fragrance industry and fragrance regulators, and the experts consider that: the essential oil of the Filipendula officinalis extracted by the invention is warm and sweet, caramel, light green, light herb and fruity paste fragrance, has a fragrance type, a delicate fragrance type, a rose fragrance type and a herb type, has fresh, natural and powerful whole fragrance, and is a novel fragrance raw material in daily chemical blending.

The invention adopts the dynamic and static leaching and the leaching extraction process of the flower bed fixed solvent circulation to extract the Filipendula vulgaris extract, has simple process and equipment, less investment, no waste of raw materials, low cost, good extract quality and high yield, and the extract yield can reach 0.48 percent.

Drawings

FIG. 1 is a flow chart of the method for extracting Filipendula vulgaris extract according to the present invention.

Detailed Description

As shown in figure 1, the method for extracting the Filipendula ulmaria extract mainly adopts a dynamic and static leaching and bed fixed solvent circulating leaching extraction process to prepare the Filipendula ulmaria extract, and is realized by the following steps:

step one, raw material pretreatment

And (4) harvesting the mosquito raw material when 70% of flowers of the mosquito are open in 6-7 months, and removing withered leaves and thick stalks at the lower part.

And step two, putting the raw materials into the flower columns, wherein the materials are required to be uniformly charged, weighing, and charging 300-350 kg in each tank, wherein the upper flower column and the lower flower column are one tank.

And step three, putting the flower column into the leaching tank by using the electric hoist.

Step four, injecting petroleum ether with a boiling range of 60-70 ℃ into the storage tank, wherein the material-liquid ratio is as follows: the raw material, petroleum ether, is 1: 3.

And step five, statically soaking for 2.5 hours, then opening a valve of a circulating system, starting the circulating pump to circulate for 30 minutes, and then circulating once every 1 hour for six hours in total and circulating for three times.

Step six, after leaching, pumping the leaching liquor into a concentration tank, washing residues twice by using petroleum ether, wherein the using amount of the petroleum ether in each time is the same, and the volume ratio is as follows: the leaching liquor is petroleum ether with the ratio of 1:2.5, and the washing time is 30 minutes respectively.

In order to save energy, the washing liquid is respectively used as the immersion liquid and the washing liquid of the next raw material, and the process is as follows:

fresh petroleum ether, secondary washing, primary washing, leaching and leaching liquor.

Seventhly, controlling the solvent in the residues in the leaching tank to be clean, closing a circulating system, opening a distillation system, introducing steam into the leaching tank for 30 minutes, and blowing out residual petroleum ether; cooling the blown petroleum ether, and then pumping the cooled petroleum ether into a reaction pot for deodorization treatment, wherein the petroleum ether can be recycled after treatment.

And step eight, opening a steam switch of the falling film evaporator, and controlling a pressure gauge to be 0.1 Mpa.

And step nine, opening a valve of the concentration tank for concentration, and condensing the solvent through a condenser to enter a storage tank for reuse.

And step ten, controlling the concentration speed, finishing concentration within two hours, and concentrating to 3-5 liters of concentrated solution.

Step eleven, filtering the concentrated solution, and carrying out reduced pressure concentration in a 3-5L flask until petroleum ether completely flows out.

And step twelve, adding absolute ethyl alcohol, and continuously concentrating until the solvent does not drip out.

And step thirteen, discharging, and cooling to room temperature to obtain a dark green paste.

And step fourteen, weighing, bottling and warehousing.

Example 1 determination of optimum test conditions

Production equipment

(1) Leaching tank: two flower columns are arranged in the device and are used for extracting effective ingredients in the raw materials;

(2) a solvent storage tank: for storing the solvent;

(3) circulating pump: for solvent circulation;

(4) a head tank: for storing the leach liquor;

(5) a falling film evaporator: evaporating the solvent and concentrating the extract;

(6) a condenser: for condensation of the solvent;

(7) receiving a bottle: a concentrate is received.

Second, the experimental contents

1. Influence of harvesting time on extract yield

(1) Purpose of the experiment: the best recovery time is determined through experiments, and the highest extract extraction yield is obtained.

(2) The experimental method comprises the following steps: three growth stages are designed, and extract extraction is respectively carried out.

(3) The experimental contents are as follows: the growth stages are divided as follows: early flowering, flowering and fruit stage.

(4) The results are shown in Table 1.

TABLE 1 Effect of harvest time on extract yield

As can be seen from the table above, the yield of the extract extracted in the flowering phase is highest in the harvesting time, and the yield in the fruit phase is only second, so that the fluid can be harvested in both the flowering phase and the fruit phase. According to experimental data, the harvest season of the Filipendula esculenta is preferably arranged from 7 to august.

2. Determination of extract content of different parts

(1) Purpose of the experiment: the content of the extractum at different parts is determined by tests.

(2) The experimental method comprises the following steps: four growth stages are designed, and the extractum is extracted respectively.

(3) The experimental contents are as follows: selecting the leaves, flowers, stems and whole plants of the Filipendula ulmaria to extract the extractum respectively.

(4) The results are shown in Table 2.

TABLE 2 determination of extract content at different sites

	Leaf of Chinese character	Stem of a tree	Flower (A. B. A. B. A. B. A. B. A. B. A. B. A. B. A. B. A. B. A. B. A. B. A. B. A. B. A. B. A. B. A. B. A	Whole plant
					Weight (kg)	30	25	40	60
De oil (g)	180	20	320	246
					Yield (%)	0.6	0.08	0.8	0.41

As can be seen from the comparison of the data in Table 2, the extract content is highest in flower, lowest in leaf and lowest in stem. Therefore, during extraction, part of thick stems can be removed, so that the content of the extract is improved, and the economic benefit is improved.

3. Influence of extraction time and extraction mode on extract

Fresh Filipendula ulmaria raw material is put into three leaching tanks respectively, each 100kg, and petroleum ether is added to make the raw material submerged (the dosage is about 500L).

The test scheme is as follows: tank I: the solution is statically immersed for 24 hours. Tank II: and (5) carrying out dynamic immersion for 3 hours. Tank No. iii: the immersion was carried out for 2 hours and then cycled every 1 hour for 30 minutes for a total of six hours (three cycles for 1.5 hours). And (4) after the completion, cleaning the leaching liquor, washing the residual residues with new petroleum ether twice respectively, and pumping the washing liquor into respective leaching liquor for concentration and refining to obtain extract. The test was repeated twice, and the results are shown in Table 3.

TABLE 3 comparative table of leaching mode

From the data in table 3, it can be seen that: the static leaching yield is higher, but the leaching time is too long, which is not beneficial to the industrialized production. The dynamic leaching time is shorter, but the yield is low and uneconomical. The dynamic and static combination has obvious advantages in yield and time, is economical and time-saving, and therefore, the dynamic and static combination in the production is better. That is, the immersion is performed for 2 hours, and then the immersion is performed every 1 hour for 30 minutes for a total of six hours (the total time of the three times of immersion is 1.5 hours).

Example 2 extraction of Filipendula extract

Step one, raw material pretreatment

And step two, putting the raw materials into the flower columns, wherein the materials are required to be uniformly charged, weighing, and charging 300 kg in each tank, wherein the upper flower column and the lower flower column are one tank.

Step four, injecting petroleum ether with the boiling range of 60 ℃ into the storage tank, and adding 900 liters of petroleum ether.

And step six, after leaching, pumping the leaching liquor into a concentration tank, washing residues twice by using petroleum ether, and adding 750 liters of petroleum ether for washing each time for 30 minutes.

Seventhly, completely controlling petroleum ether in the residues in the leaching tank, closing a circulating system, opening a distillation system, introducing steam into the leaching tank for 30 minutes, and blowing out the residual petroleum ether; cooling the blown petroleum ether, and then pumping the cooled petroleum ether into a reaction pot for deodorization treatment, wherein the petroleum ether can be recycled after treatment.

And step ten, controlling the concentration speed, finishing the concentration within two hours, and concentrating to 3 liters of concentrated solution.

Step eleven, filtering the concentrated solution, and concentrating the concentrated solution in a 3L flask under reduced pressure until petroleum ether is drained.

And step fourteen, weighing, bottling and warehousing.

Example 3 extraction of Filipendula extract

Step one, raw material pretreatment

And step two, putting the raw materials into the flower columns, wherein the materials are required to be uniformly charged, weighing, wherein the upper flower column and the lower flower column are a tank, and 330 kg of materials are charged in each tank.

Step four, injecting petroleum ether with the boiling range of 65 ℃ into the storage tank, and adding 990 liters of petroleum ether.

And step six, after the leaching is finished, pumping the leaching liquor into a concentration tank, washing residues twice by using petroleum ether, and adding 780 liters of petroleum ether for washing each time for 30 minutes.

And step ten, controlling the concentration speed, finishing the concentration within two hours, and concentrating to 4 liters of concentrated solution.

Step eleven, filtering the concentrated solution, and concentrating the concentrated solution in a 4L flask under reduced pressure until petroleum ether is drained.

And step fourteen, weighing, bottling and warehousing.

Example 4 extraction of Filipendula extract

Step one, raw material pretreatment

And step two, putting the raw materials into the flower columns, wherein the materials are required to be uniformly charged, weighing, wherein the upper flower column and the lower flower column are a tank, and each tank is charged with 350 kg.

Step four, injecting petroleum ether with the boiling range of 70 ℃ into the storage tank, and adding 1050 liters of petroleum ether.

And step six, after leaching, pumping the leaching liquor into a concentration tank, washing residues twice by using petroleum ether, and adding 870 liters of petroleum ether for washing each time for 30 minutes.

And step ten, controlling the concentration speed, finishing the concentration within two hours, and concentrating to 5 liters of concentrated solution.

Step eleven, filtering the concentrated solution, and concentrating the concentrated solution in a 5L flask under reduced pressure until petroleum ether is drained.

And step fourteen, weighing, bottling and warehousing.

Statistics are made on the extract yields of examples 2-4, and the results are shown in Table 4.

TABLE 4

Item	Extract yield (%)
		Example 2	0.48
Example 3	0.49
		Example 4	0.47
Comparative example (conventional solvent extraction method)	0.35

The data in the table show that when the extracting method is used for extracting the Filipendula ulmaria extract, the extract yield is as follows: 0.48 percent.

The mosquito extract is a novel spice, is sold at home and abroad, is temporarily set to be 1000 yuan/kg according to the lilac extract (1600 yuan/kg), the lily of the valley extract (2400 yuan/kg), the pine needle extract (1000 yuan/kg) and actual production consumption (see table 5), and can be profitable for 589.7 yuan per kg.

TABLE 5 cost per kg of extract

Consumption item	Quantity (kg)	Monovalent (Yuan/kg)	Amount (Yuan)
				Raw materials	80	0.32	25.6
Petroleum ether	70	2.6	182
				Water (W)			5
Electric power			22
				Coal (coal)			45.7
Ethanol			20
				Payroll			39
Others (repair, depreciation, management)			80
				Total up to			419.3

The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims

1. The method for extracting the herba Filipendulae extract is characterized by comprising the following steps of:

step one, raw material pretreatment

step two, putting the raw materials into the flower columns, wherein the materials are required to be uniformly charged, weighing, wherein the upper flower column and the lower flower column are a tank, and 330 kg of materials are charged in each tank;

step four, injecting petroleum ether with a boiling range of 65 ℃ into the storage tank, and adding 990 liters of petroleum ether;

step six, after leaching, pumping the leaching liquor into a concentration tank, washing residues twice by using petroleum ether, and adding 780 liters of petroleum ether for washing each time for 30 minutes;

seventhly, completely controlling petroleum ether in the residues in the leaching tank, closing a circulating system, opening a distillation system, introducing steam into the leaching tank for 30 minutes, and blowing out the residual petroleum ether; cooling the blown petroleum ether, and then pumping the cooled petroleum ether into a reaction pot for deodorization treatment, wherein the petroleum ether can be recycled after treatment;

step ten, controlling the concentration speed, completing the concentration within two hours, and concentrating to 4 liters of concentrated solution;

step eleven, filtering the concentrated solution, and carrying out reduced pressure concentration in a 4L flask until petroleum ether completely flows out;

thirteen, discharging, cooling to room temperature to obtain dark green paste;

and step fourteen, weighing, bottling and warehousing.