CN109293711A - A method of Lilium brownie class compound is extracted using Simulation moving bed - Google Patents

A method of Lilium brownie class compound is extracted using Simulation moving bed Download PDF

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Publication number
CN109293711A
CN109293711A CN201811156841.6A CN201811156841A CN109293711A CN 109293711 A CN109293711 A CN 109293711A CN 201811156841 A CN201811156841 A CN 201811156841A CN 109293711 A CN109293711 A CN 109293711A
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China
Prior art keywords
moving bed
simulation moving
follows
motor
class compound
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CN201811156841.6A
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傅春燕
刘永辉
粟雯
何芳
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Shaoyang University
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Shaoyang University
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07GCOMPOUNDS OF UNKNOWN CONSTITUTION
    • C07G3/00Glycosides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0207Control systems

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Automation & Control Theory (AREA)
  • Management, Administration, Business Operations System, And Electronic Commerce (AREA)

Abstract

The invention belongs to technical field of biological extraction, disclose a kind of method for extracting Lilium brownie class compound using Simulation moving bed, the method for extracting Lilium brownie class compound using Simulation moving bed are as follows: using lily bulb as raw material, new fresh lily bulb is cleaned into stripping valve, 1h is steamed under 100 DEG C of high steam, is cooled to room temperature and is spontaneously dried, it is 10% or so to moisture content, after being crushed with pulverizer, 60 meshes are crossed, it is spare;It takes 10g or more lily root flour to be added in 80% ethanol solution and impregnates 48h, flow back 12h at 60 DEG C, filters, residue is added alcohol reflux again, filters, filtrate is merged;The above filtrate is extracted into saponins compound by Simulation moving bed.The saponins compound in lily is precipitated completely in the present invention, greatly improves the purity of saponins compound, and extraction process is pollution-free, without the participation of any other solvent, avoids the separation to other substances, easy to operate.

Description

A method of Lilium brownie class compound is extracted using Simulation moving bed
Technical field
The invention belongs to technical field of biological extraction more particularly to a kind of utilization Simulation moving bed to extract Lilium brownie class The method for closing object.
Background technique
Saponin(e (Saponin) nickname: alkali soap body;Saponin;Saponin (zaodai);Saponin;Or saponarin." saponin(e " word From English name Saponin free translation, English name is then derived from Latin Sapo, means soap.Saponin(e (Saponin) is aglycon For triterpene or a kind of glucosides of spirostane class compound, it is distributed mainly in the higher plant of land, is also present in starfish on a small quantity In the marine organisms such as sea cucumber.The principle active component of many Chinese herbal medicines such as ginseng, Radix Polygalae, campanulaceae, Radix Glycyrrhizae, rhizoma anemarrhenae and radix bupleuri etc. All contain saponin(e.Some saponin(es also have the valuable bioactivity such as the active or antipyretic, calm of antibacterial, anticancer.Saponin(e In chemical structure, since aglycon has different degrees of lipophilicity, sugar chain has stronger hydrophily, and saponin(e is made to become a kind of table Face activating agent can generate persistent soap sample foam after aqueous solution shaking.Some plant extracts rich in saponin(e are used for Manufacture emulsifier, abluent and foaming agent etc..However, during the existing extraction Lilium brownie class compound using Simulation moving bed Pressure detection data error is big, influences to extract quality;Meanwhile existing heating is uneven, causes to extract Lilium brownie class chemical combination substance It is poor to measure.
In conclusion problem of the existing technology is:
(1) DNA purity of traditional saponin compound summarized to lily is lower, and operation is more complex, needs many kinds of substance It extracts, causes separation difficult, reduce the rate of recovery of saponins compound.
(2) for traditional central control unit to the control of each device there are error, the load parameter of server is more, it is difficult to Optimal resource allocation is carried out to each device, reduces working efficiency.
Summary of the invention
In view of the problems of the existing technology, Lilium brownie class is extracted using Simulation moving bed the present invention provides a kind of The method for closing object.
The invention is realized in this way a method of Lilium brownie class compound is extracted using Simulation moving bed are as follows:
Using lily bulb as raw material, processing step is as follows:
Step 1: new fresh lily bulb is cleaned into stripping valve, 1h is steamed under 100 DEG C of high steam, is cooled to room temperature carry out nature It is dry, until moisture content is 10% or so, after being crushed with pulverizer, 60 meshes are crossed, it is spare;
The pulverizer combination fuzzy-adaptation PID control, using the static characteristic Controlling model of pulverizer motor;Motor obscures The stable state of PID adaptive Gaussian filtering exports are as follows:
Wherein, kpFor the spinner velocity ring of motor, kiError, the cascade positioning of motor are controlled for three-phase balance state Electric current loop indicates are as follows:
PID controller, stepper motor undamped nonlinear ionization transmission control system are adjusted using circulation tracking stepping method System is adjusted using PID controller, the output of controller are as follows:
In formula, LqIndicate the drunk power tracking change rate of motor, UJIndicate the time of integration, UEWhen being the differential of PID control Between;Control error feedback, output are carried out by way of linear combination are as follows:
Δ v (l)=LQΔf(l)+LJf(l)+LE[Δf(l)-Δf(l-1)].
Wherein, LqIndicate sample rate current,It is the integral parameter of motor control,It is stepping The differential parameter of motor control;
Step 2: taking 10g or more lily root flour to be added in 80% ethanol solution and impregnate 48h, and flow back 12h at 60 DEG C, filters, Residue is added into alcohol reflux again, filters, filtrate is merged;
Step 3: the above filtrate is extracted into saponins compound by Simulation moving bed.
Further, the condition that the Simulation moving bed extracts are as follows: stationary phase is to choose from Germany MERCKLiChroprepNH2Preparation scale filler;Mobile phase is that volume fraction is 95% methanol solution.
Further, the tubing string of the Simulation moving bed is 8, is the stainless-steel tubing pillar of diameter 10mm, length 15cm, I Band flow velocity is 2ml/min, and II band flow velocity is 2ml/min, and III band flow velocity is 1ml/min, and IV band flow velocity is 3ml/min, sample introduction stream Speed is 2ml/h, switching time 8min.
Further, the simulated moving bed system is provided with central control unit, solenoid valve, flowmeter, PLC program control System pump.
Further, the central control unit realizes the analysis to each module using the LBFA algorithm based on cloud computing system With regulation, the process of LBFA algorithm are as follows:
(1) position (X, Y) of the center of gravity G of the current phase space projection method of cloud computing system is calculated;
(2) current load value (load vector (a, b)) is received;
(3) it calculates and is located at the Δ LB value that system after present load is assigned in optimal phase subspace interior joint in phase space;
(4) it chooses the smallest node of current Δ LB and carries out task distribution, the system load balancing degree LB after guaranteeing distribution is most It is small;
(5) system position of centre of gravity current in phase space is recalculated, according to formulaUtilize this The load value of distribution directly calculates new position of centre of gravity;
(6) (2) are returned to and starts new assigning process.
Advantages of the present invention and good effect are as follows: the present invention by lily carry out thermophilic digestion pretreatment, and further It is filtered to being impregnated in lily again ethyl alcohol, the saponins compound in lily is precipitated completely, by using simulated moving bed system Saponins compound is extracted, the purity of saponins compound is greatly improved, extraction process is pollution-free, not any The participation of other solvents avoids the separation to other substances, easy to operate.
Central control unit by using the LBFA algorithm based on cloud computing system meet under the conditions of great deal of nodes into Row scheduling of resource task improves the efficiency and purity of extraction.
Detailed description of the invention
Fig. 1 is the method flow diagram that Lilium brownie class compound is extracted using Simulation moving bed that the present invention implements to provide.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to Limit the present invention.
With reference to the accompanying drawing and specific embodiment is further described application principle of the invention.
As shown in Figure 1, the method provided in an embodiment of the present invention for extracting Lilium brownie class compound using Simulation moving bed The following steps are included:
S101: new fresh lily bulb is cleaned into stripping valve, steams 1h under 100 DEG C of high steam, it is dry to be cooled to room temperature progress nature It is dry, until moisture content is 10% or so, after being crushed with pulverizer, 60 meshes are crossed, it is spare;
S102: taking 10g or more lily root flour to be added in 80% ethanol solution and impregnate 48h, and flow back 12h at 60 DEG C, filters, will Residue adds alcohol reflux again, filters, filtrate is merged;
S103: the above filtrate is extracted into saponins compound by Simulation moving bed.
The pulverizer combination fuzzy-adaptation PID control, using the static characteristic Controlling model of pulverizer motor;Motor obscures The stable state of PID adaptive Gaussian filtering exports are as follows:
Wherein, kpFor the spinner velocity ring of motor, kiError, the cascade positioning of motor are controlled for three-phase balance state Electric current loop indicates are as follows:
PID controller, stepper motor undamped nonlinear ionization transmission control system are adjusted using circulation tracking stepping method System is adjusted using PID controller, the output of controller are as follows:
In formula, LqIndicate the drunk power tracking change rate of motor, UJIndicate the time of integration, UEWhen being the differential of PID control Between;Control error feedback, output are carried out by way of linear combination are as follows:
Δ v (l)=LQΔf(l)+LJf(l)+LE[Δf(l)-Δf(l-1)];
Wherein, LqIndicate sample rate current,It is the integral parameter of motor control,It is step Into the differential parameter of motor control;
The condition that Simulation moving bed provided in an embodiment of the present invention extracts are as follows:
Stationary phase used is to choose from Germany MERCKLiChroprepNH2Preparation scale filler;Mobile phase is volume fraction For 95% methanol solution.
The tubing string of Simulation moving bed provided in an embodiment of the present invention is 8, is the stainless steel of diameter 10mm, length 15cm Tubing string, I band flow velocity are 2ml/min, and II band flow velocity is 2ml/min, and III band flow velocity is 1ml/min, and IV band flow velocity is 3ml/min, Sample introduction flow velocity is 2ml/h, switching time 8min.
Simulated moving bed system provided in an embodiment of the present invention is provided with central control unit, solenoid valve, flowmeter, PLC Process control pump.
Central control unit provided in an embodiment of the present invention is realized using the LBFA algorithm based on cloud computing system to each mould The analysis and regulation of block, the process of LBFA algorithm are as follows:
(1) position (X, Y) of the center of gravity G of the current phase space projection method of cloud computing system is calculated;
(2) current load value (load vector (a, b)) is received;
(3) it calculates and is located at the Δ LB value that system after present load is assigned in optimal phase subspace interior joint in phase space;
(4) it chooses the smallest node of current Δ LB and carries out task distribution, the system load balancing degree LB after guaranteeing distribution is most It is small;
(5) system position of centre of gravity current in phase space is recalculated, according to formulaUtilize this The load value of distribution directly calculates new position of centre of gravity;
(6) (2) are returned to and starts new assigning process;
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.

Claims (5)

1. a kind of method for extracting Lilium brownie class compound using Simulation moving bed, which is characterized in that described to be moved using simulation The method that dynamic bed extracts Lilium brownie class compound are as follows:
Step 1: lily is cleaned into stripping valve, 1h is steamed under 100 DEG C of high steam, is cooled to room temperature and is spontaneously dried, until containing Water rate is 10%, after being crushed with pulverizer, crosses 60 meshes, spare;
The pulverizer combination fuzzy-adaptation PID control, using the static characteristic Controlling model of pulverizer motor;The fuzzy of motor The stable state of adaptive Gaussian filtering exports are as follows:
Wherein, kpFor the spinner velocity ring of motor, kiError, the cascade location current of motor are controlled for three-phase balance state Ring indicates are as follows:
PID controller, stepper motor undamped nonlinear ionization driving control system benefit are adjusted using circulation tracking stepping method It is adjusted with PID controller, the output of controller are as follows:
In formula, LqIndicate the drunk power tracking change rate of motor, UJIndicate the time of integration, UEIt is the derivative time of PID control; Control error feedback, output are carried out by way of linear combination are as follows:
Δ v (l)=LQΔf(l)+LJf(l)+LE[Δf(l)-Δf(l-1)];
Wherein, LqIndicate sample rate current,It is the integral parameter of motor control,It is stepper motor The differential parameter of control;
Step 2: taking 10g or more lily root flour to be added in 80% ethanol solution and impregnate 48h, and flow back 12h at 60 DEG C, filters, will be residual Slag adds alcohol reflux again, filters, filtrate is merged;
Step 3: the above filtrate is extracted into saponins compound by Simulation moving bed.
2. the method for extracting Lilium brownie class compound using Simulation moving bed as described in claim 1, which is characterized in that described The condition that Simulation moving bed extracts are as follows: stationary phase is preparation scale filler;Mobile phase is that volume fraction is 95% methanol solution.
3. the method for extracting Lilium brownie class compound using Simulation moving bed as described in claim 1, which is characterized in that described The tubing string of Simulation moving bed is 8, is the stainless-steel tubing pillar of diameter 10mm, length 15cm, I band flow velocity is 2ml/min, II band Flow velocity is 2ml/min, and III band flow velocity is 1ml/min, and IV band flow velocity is 3mi/min, and sample introduction flow velocity is 2ml/h, and switching time is 8min。
4. the method for extracting Lilium brownie class compound using Simulation moving bed as described in claim 1, which is characterized in that described Simulated moving bed system is provided with central control unit, solenoid valve, flowmeter, PLC program control pump.
5. simulated moving bed system as claimed in claim 4, which is characterized in that the central control unit, which uses, is based on cloud computing The LBFA algorithm of system realizes the analysis and regulation to each module, the process of LBFA algorithm are as follows:
(1) position (X, Y) of the center of gravity G of the current phase space projection method of cloud computing system is calculated;
(2) current load value (load vector (a, b)) is received;
(3) it calculates and is located at the Δ LB value that system after present load is assigned in optimal phase subspace interior joint in phase space;
(4) it chooses the smallest node of current Δ LB and carries out task distribution, the system load balancing degree LB after guaranteeing distribution is minimum;
(5) system position of centre of gravity current in phase space is recalculated, according to formulaUtilize this sub-distribution Load value directly calculate new position of centre of gravity;
(6) (2) are returned to and starts new assigning process.
CN201811156841.6A 2018-09-30 2018-09-30 A method of Lilium brownie class compound is extracted using Simulation moving bed Pending CN109293711A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101628075A (en) * 2009-06-22 2010-01-20 包头市千年健药物研究开发有限公司 Method for preparing lilium total saponin extract by using macroporous resin and application thereof
CN101781351A (en) * 2009-01-21 2010-07-21 重庆华森制药有限公司 Method for extracting ginsenoside Rb1 from American ginseng and powder-injection thereof
CN102336799A (en) * 2010-07-22 2012-02-01 辽宁科技大学 Simulated moving bed chromatography separation method for preparing ginsenoside Rb1
CN104193793A (en) * 2014-08-07 2014-12-10 中国农业科学院特产研究所 Method for preparing ginsenoside Rb3 in American ginseng fruit by adopting simulated moving bed
CN107412546A (en) * 2017-07-14 2017-12-01 百色学院 A kind of method of Lilium lancifo1ium Thunb extraction saponin(e
CN107661365A (en) * 2017-09-22 2018-02-06 右江民族医学院 The method for extracting luffa total saposins

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101781351A (en) * 2009-01-21 2010-07-21 重庆华森制药有限公司 Method for extracting ginsenoside Rb1 from American ginseng and powder-injection thereof
CN101628075A (en) * 2009-06-22 2010-01-20 包头市千年健药物研究开发有限公司 Method for preparing lilium total saponin extract by using macroporous resin and application thereof
CN102336799A (en) * 2010-07-22 2012-02-01 辽宁科技大学 Simulated moving bed chromatography separation method for preparing ginsenoside Rb1
CN104193793A (en) * 2014-08-07 2014-12-10 中国农业科学院特产研究所 Method for preparing ginsenoside Rb3 in American ginseng fruit by adopting simulated moving bed
CN107412546A (en) * 2017-07-14 2017-12-01 百色学院 A kind of method of Lilium lancifo1ium Thunb extraction saponin(e
CN107661365A (en) * 2017-09-22 2018-02-06 右江民族医学院 The method for extracting luffa total saposins

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
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Application publication date: 20190201