CN105153274A - Method for removing heavy metal by electrodialysis method during hirudin extraction production - Google Patents
Method for removing heavy metal by electrodialysis method during hirudin extraction production Download PDFInfo
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- CN105153274A CN105153274A CN201510542702.7A CN201510542702A CN105153274A CN 105153274 A CN105153274 A CN 105153274A CN 201510542702 A CN201510542702 A CN 201510542702A CN 105153274 A CN105153274 A CN 105153274A
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Abstract
The invention discloses a method for removing heavy metal by electrodialysis method during hirudin extraction production. The method includes the steps of preprocessing leeches, subjecting the preprocessed leeches to uniform smashing, centrifugal separation and insoluble substance filtering to obtain a hirudin liquid mixture, adding acid into the mixture to reduce pH value and dilute the hirudin liquid relatively, feeding the mixture to electrodialysis equipment while setting appropriate current intensity to protect bioactivity of hirudin, removing heavy metal such as lead under action of ion rejection in electrodialysis after reflux circulating for a certain time, then dewatering treated liquid by means of nanofiltration membrane until concentration of the liquid is moderate, and finally pulverizing after spray drying or directly making the liquid into a hirudin liquid product. By the method, the problem that content of heavy metal such as lead in finished products obtained from thirudin extraction production is too high, which brings bad influence to application of downstream firms is solved. Besides, chemical medicine consumption is omitted from the method while production process is simplified and production cost is reduced.
Description
Technical field
The present invention relates to a kind of electroosmose process adopted in electrochemical means, extracting in natural hirudin production process from leech, remove the heavy metal contained by r-hirudin, to obtain the production method of pure leech extract.
Background technology
R-hirudin (hirudin) obtains because being separated from leech the earliest and gaining the name.Natural hirudin is made up of 65 amino-acid residues, molecular weight 7000 dalton.It is the most strong thrombin inhibitors found in current nature animal body.R-hirudin also has very strong anti thrombotic action, for various thrombus disease as phlebothrombosis, disseminated inravascular coagulation, brain blood coagulation, thrombophlebitis and coronary artery thrombosis have prevention and therapy effect, the especially treatment of phlebothrombosis and disseminated intravascular coagulation; Also can be used for the formation of surgical site infections prevention of arterial thrombus, prevention thrombus after or postangioplasty embolism again; Improve extracorporeal circulation of blood and blood dialysis, Chang Yinwei anastomosis blood vessel embolism in microsurgery and leading to the failure, adopt r-hirudin to promote wound healing.R-hirudin is as the natural animal peptide class with anti-freezing, anti-thrombus function, can improve blood of human body follow system Working environment, improve its working efficiency, the conveying of promotion needed by human body nutrient and medicine are to effective covering of focus, so r-hirudin has important effect to the health of the mankind and health care.
The r-hirudin separated from leech at present, because of the impact of the growing environment of leech and the factor of extraction processing aspect, be found with heavy metals such as lead, make it that people can be caused in actual applications to occur the problem of health and safety aspect, thus constrain its application.Leaded general > 2 mg/kg dry powder (500AT-U/g dry powder sample) in the r-hirudin of current volume production, because heavy metal can not decompose destruction, their position can only be shifted or change their physics or chemical form, so removing heavy metal process in, the method that can not affect the condition of pending thing be do not allow detectable.Current removal heavy metal has had employing ion exchange method, but the resin related to is of a great variety, and actual effect is also not obvious, and cost is higher, pending thing effective efficiency component damages also can be made excessive, not feasible economically simultaneously.Electroosmose process refers under the effect of applying direct current electric field, utilize the selective penetrated property of anion-exchange membrane and cationic exchange membrane, make a part of ion permeable exchange membrane and move in another part water, thus make the process that a part of water is desalinated and another part water is concentrated, electrodialysis belongs to ion rejection displacement, ion-exchange membrane plays ion selective during the course and cuts resistance effect, so or rather, ion-exchange membrane should be called that ion selectivity is through film, do not need to consume pharmaceutical chemicals, equipment is simple, easy to operate, is applicable to continuous seepage and uses.Use electroosmose process effectively can remove the heavy metals such as delead in the extraction of r-hirudin is produced, to simplifying production technique, reduce production cost, the application that this technology is produced at r-hirudin has no report.
Summary of the invention
A kind of electroosmose process is the object of the present invention is to provide to extract the method for removal heavy metal in production at r-hirudin.
In order to achieve the above object, the present invention takes following steps:
Step 1, pre-treatment: freeze the slow impurity melting leech rinsed with deionized water 1 ~ 20 minute removing leech surface of freezing treatment by slow;
Step 2, homogeneous is pulverized: static 20 ~ 90 minutes of the sodium chloride solution putting into 0.2 ~ 1% of 0.5 ~ 1.2 times of weight, through colloidal mill high speed pulverization, Homogenizing pump homogeneous;
Step 3, centrifugation: add 0.005 ~ 0.05% trehalose, 0.005 ~ 0.02% acetyl half wing propylhomoserin, 0.005 ~ 0.05% matrimony vine acid sodium and 0.1 ~ 0.75 sodium-chlor mixed stabilizer; Be that 120000 revs/min of whizzers carry out solid-liquid separation at rotating speed;
Step 4, add acid and reduce pH value: liquid state mutually in add the hydrochloric acid liquid of 0.5 ~ 3 times amount, adjustment mixed solution pH value is 4.5 ~ 6.8;
Step 5, heavy-metal ion removal: pump into electrodialysis module group, machine internal recycle 0.5 ~ 4 hour, through electrodialytic ion rejection effect heavy-metal ion removal;
Step 6, eventually pass 800 μm of nanofiltration membrane subsequent disposal and remove 20% ~ 50% moisture in 30 ~ 180 minutes, then add the medical starch of weight ratio 1% ~ 15%, 100 ~ 180 degrees Celsius of spraying dry can be made into the Iirudo-seu-whitmania essence containing antithrombin activity 400 ~ 2000AT-U/g.
Preferably, in step 4, the pH value adding 3 times amount is 4.5 hydrochloric acid liquid; In steps of 5, the machine internal recycle time is 0.5 ~ 2 hour; In step 6, the medical starch adding weight ratio 1% ~ 15% is excipient, can be made into the r-hirudin lyophilized powder finished product containing antithrombin activity 800 ~ 2000AT-U/g through negative pressure lyophilize.
The present invention has following beneficial effect: the invention solves at present in other r-hirudin extraction process finished product the plumbous heavy metal content too high (general > 2 mg/kg dry powder (800AT-U/g dry powder sample)) that waits be unfavorable for the problem that down-stream enterprise applies, the method does not need to consume pharmaceutical chemicals, simplify production technique, reduce production cost.
Embodiment
Be clearly and completely described the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
Electroosmose process extracts a method for removal heavy metal in production at r-hirudin, comprises the following steps:
Step 1, pre-treatment: freeze the slow impurity melting leech rinsed with deionized water 1 ~ 20 minute removing leech surface of freezing treatment by slow;
Step 2, homogeneous is pulverized: static 20 ~ 90 minutes of the sodium chloride solution putting into 0.2 ~ 1% of 0.5 ~ 1.2 times of weight, through colloidal mill high speed pulverization, Homogenizing pump homogeneous;
Step 3, centrifugation: add 0.005 ~ 0.05% trehalose, 0.005 ~ 0.02% acetyl half wing propylhomoserin, 0.005 ~ 0.05% matrimony vine acid sodium and 0.1 ~ 0.75 sodium-chlor mixed stabilizer; After mixing, be that 120000 revs/min of whizzers carry out solid-liquid separation through rotating speed;
Step 4, add acid and reduce pH value: liquid state mutually in add the hydrochloric acid liquid of 0.5 times amount, adjustment mixed solution pH value is 4.5 ~ 6.8;
Step 5, heavy-metal ion removal: pump into electrodialysis module group, electrodialysis anode commonly uses graphite, material; Negative electrode can be made with materials such as stainless steels, and processing power selects the industrialized standard equipment of 1 ~ 3 ton/day, and machine internal recycle 1 ~ 4 hour, through electrodialytic ion rejection effect heavy-metal ion removal;
Step 6, eventually pass 800 μm of nanofiltration membrane subsequent disposal and remove 20% ~ 50% moisture in 30 ~ 180 minutes, then add the medical starch of weight ratio 1% ~ 13%, 100 ~ 180 degrees Celsius of spraying dry can be made into the Iirudo-seu-whitmania essence finished product containing antithrombin activity 400 ~ 1000AT-U/g.Iirudo-seu-whitmania essence finished product of the present invention is leaded waits heavy metal content < 0.002 mg/kg dry powder.
Embodiment 2
Electroosmose process extracts a method for removal heavy metal in production at r-hirudin, comprises the following steps:
Step 1, pre-treatment: freeze the slow impurity melting leech rinsed with deionized water 1 ~ 20 minute removing leech surface of freezing treatment by slow;
Step 2, homogeneous is pulverized: static 20 ~ 90 minutes of the sodium chloride solution putting into 0.2 ~ 1% of 0.5 ~ 1.2 times of weight, through colloidal mill high speed pulverization, Homogenizing pump homogeneous;
Step 3, centrifugation: add 0.005 ~ 0.05% trehalose, 0.005 ~ 0.02% acetyl half wing propylhomoserin, 0.005 ~ 0.05% matrimony vine acid sodium and 0.1 ~ 0.75 sodium-chlor mixed stabilizer; After mixing, be that 120000 revs/min of whizzers carry out solid-liquid separation through rotating speed;
Step 4, add acid and reduce pH value: liquid state mutually in add the hydrochloric acid liquid of 3 times amount, adjustment mixed solution pH value is 4.5;
Step 5, heavy-metal ion removal: pump into electrodialysis module group, electrodialysis anode commonly uses graphite, material; Negative electrode can be made with materials such as stainless steels, and processing power selects the industrialized standard equipment of 1 ~ 3 ton/day, and machine internal recycle 0.5 ~ 2 hour, through electrodialytic ion rejection effect heavy-metal ion removal;
Step 6, eventually pass 800 μm of nanofiltration membrane subsequent disposal and remove 20% ~ 50% moisture in 30 ~ 180 minutes, then add the medical starch of weight ratio 1% ~ 15%, can be made into the Iirudo-seu-whitmania essence finished product containing antithrombin activity 800 ~ 2000AT-U/g through negative pressure lyophilize.Iirudo-seu-whitmania essence finished product of the present invention is leaded waits heavy metal content < 0.002 mg/kg dry powder
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. extract a method for removal heavy metal in production with electroosmose process at r-hirudin, it is characterized in that, comprise the following steps:
Step 1, pre-treatment: freeze the slow impurity melting leech rinsed with deionized water 1 ~ 20 minute removing leech surface of freezing treatment by slow;
Step 2, homogeneous is pulverized: static 20 ~ 90 minutes of the sodium chloride solution putting into 0.2 ~ 1% of 0.5 ~ 1.2 times of weight, through colloidal mill high speed pulverization, Homogenizing pump homogeneous;
Step 3, centrifugation: add 0.005 ~ 0.05% trehalose, 0.005 ~ 0.02% acetyl half wing propylhomoserin, 0.005 ~ 0.05% matrimony vine acid sodium and 0.1 ~ 0.75 sodium-chlor mixed stabilizer; Be that 120000 revs/min of whizzers carry out solid-liquid separation at rotating speed;
Step 4, add acid and reduce pH value: liquid state mutually in add the hydrochloric acid liquid of 0.5 ~ 3 times amount, adjustment mixed solution pH value is 4.5 ~ 6.8;
Step 5, heavy-metal ion removal: pump into electrodialysis module group, machine internal recycle 0.5 ~ 4 hour, through electrodialytic ion rejection effect heavy-metal ion removal;
Step 6, eventually pass 800 μm of nanofiltration membrane subsequent disposal and remove 20% ~ 50% moisture in 30 ~ 180 minutes, then add the medical starch of weight ratio 1% ~ 15%, 100 ~ 180 degrees Celsius of spraying dry can be made into the Iirudo-seu-whitmania essence finished product containing antithrombin activity 400 ~ 2000AT-U/g.
2. electroosmose process according to claim 1 extracts the method for removal heavy metal in production at r-hirudin, and it is characterized in that: in step 4, the pH value adding 3 times amount is 4.5 hydrochloric acid liquid; In steps of 5, the machine internal recycle time is 0.5 ~ 2 hour; In step 6, the medical starch adding weight ratio 1% ~ 15% is excipient, can be made into the r-hirudin lyophilized powder finished product containing antithrombin activity 800 ~ 2000AT-U/g through negative pressure lyophilize.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101108879A (en) * | 2007-08-03 | 2008-01-23 | 广西博泰恩生物科技有限公司 | Method for extracting active ingredient of natural leech essence |
| US20090171448A1 (en) * | 2007-04-27 | 2009-07-02 | Uri Eli | Implantable device with miniature rotating portion for energy harvesting |
| CN102146136A (en) * | 2010-12-24 | 2011-08-10 | 南宁乙翔生物科技有限公司 | Method for extracting hirudin by stimulating living leech with electricity |
| CN102153645A (en) * | 2010-12-24 | 2011-08-17 | 南宁乙翔生物科技有限公司 | Method for removing heavy metal ions in hirudin by using electro-osmosis |
| CN102964446A (en) * | 2012-11-28 | 2013-03-13 | 周维官 | Method for repeatedly extracting natural hirudin from live vampire leech |
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- 2015-08-31 CN CN201510542702.7A patent/CN105153274A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090171448A1 (en) * | 2007-04-27 | 2009-07-02 | Uri Eli | Implantable device with miniature rotating portion for energy harvesting |
| CN101108879A (en) * | 2007-08-03 | 2008-01-23 | 广西博泰恩生物科技有限公司 | Method for extracting active ingredient of natural leech essence |
| CN102146136A (en) * | 2010-12-24 | 2011-08-10 | 南宁乙翔生物科技有限公司 | Method for extracting hirudin by stimulating living leech with electricity |
| CN102153645A (en) * | 2010-12-24 | 2011-08-17 | 南宁乙翔生物科技有限公司 | Method for removing heavy metal ions in hirudin by using electro-osmosis |
| CN102964446A (en) * | 2012-11-28 | 2013-03-13 | 周维官 | Method for repeatedly extracting natural hirudin from live vampire leech |
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Effective date of registration: 20180710 Address after: 530007, 3288, room 3, Kechuang building, 25-1 Keyuan Avenue, Nanning, the Guangxi Zhuang Autonomous Region. Applicant after: Nanning and Lanji Food Technology Co., Ltd. Address before: 530000 718, room 9, Hetai science and technology complex, 9 hi tech four road, the Guangxi Zhuang Autonomous Region Applicant before: Nanning Jinbei Biological Technology Co., Ltd. |
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Application publication date: 20151216 |