CN1449789A - Novel antibiotic preparation and process for preparing the same - Google Patents

Novel antibiotic preparation and process for preparing the same Download PDF

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Publication number
CN1449789A
CN1449789A CN 03112373 CN03112373A CN1449789A CN 1449789 A CN1449789 A CN 1449789A CN 03112373 CN03112373 CN 03112373 CN 03112373 A CN03112373 A CN 03112373A CN 1449789 A CN1449789 A CN 1449789A
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preparation
novel anti
raw material
ultrafiltration
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迟玉森
庄桂东
张景茹
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Abstract

The present invention relates to a novel antibiotic preparation and its preparation method. It uses the plant populus tomentosa as raw material and makes it undergo the processes of pretreatment, pulverizing, extracting, sorting and ultrafiltering, vacuum concentrating, drying and obtaining finished product. The molecular weight of its effective component is 500-4000, and the water content of said antibiotic preparation is less than 5%. It is a novel antibiotic preparation for curing infected disease due to pathogenic bacteria with resistance to broad-spectrum antibiotics of penicillin, etc.

Description

A kind of novel anti rhzomorph preparation and preparation method thereof
(1) technical field:
The present invention relates to the antibiotics technical field, is a kind of various a kind of novel anti rhzomorph preparations that broad-spectrum antibiotics such as penicillin had the caused infectious disease of chemical sproof pathogenic bacteria and preparation method thereof that are used for the treatment of specifically.
(2) background technology:
At present, when a lot of germ infectious disease of treatment, adopt antibiotics, the most frequently used is broad-spectrum antibiotics such as penicillin, use very much in a large number owing to antibiotic, make many pathogenic mushrooms possess drug resistance, even Drug resistance, thereby reduced the therapeutic effect of broad-spectrum antibiotics such as penicillin, directly influence the healthy of people, thereby a kind of being used for the treatment of variously there is a kind of antibiotic preparation of the caused infectious disease of chemical sproof pathogenic bacteria not see to broad-spectrum antibiotics such as penicillins.
(3) summary of the invention:
Purpose of the present invention is intended to overcome the deficiency of above-mentioned prior art, and a kind of various a kind of novel anti rhzomorph preparations that broad-spectrum antibiotics such as penicillin had the caused infectious disease of chemical sproof pathogenic bacteria that are used for the treatment of are provided.
Another object of the present invention provides a kind of preparation method of novel anti rhzomorph.
The present invention has mainly solved the existing problem that broad-spectrum antibiotics such as penicillin is had the therapeutic effect difference of the caused infectious disease of chemical sproof pathogenic bacteria.
In order to achieve the above object, the present invention is achieved in that a kind of novel anti rhzomorph preparation, it be by the vegetable hair Cortex Populi dividianae through pretreatment of raw material, pulverizing, lixiviate, classification ultrafiltration, vacuum concentration, drying, make finished product.
A kind of novel anti rhzomorph preparation of the present invention, its described antibiotic preparation active ingredient molecular weight is 500-4000, the water content of its described antibiotic preparation<5%.
In order to achieve the above object, the preparation method of a kind of novel anti rhzomorph preparation of the present invention comprises following processing step:
A, the pretreatment of raw material, the leaf of the Chinese white poplar bark of plucking a plant, branch, bark are cleaned and are dried the back as raw material;
B pulverizes, and above-mentioned raw materials is pulverized, and smashing fineness is the 10-30 order;
C, lixiviate with the ethanol water of 0-95%, is soaked the raw material of pulverizing, raw material with the water ratio is: the Cortex Populi Tomentosae raw material: water is 1: 3-7, extraction temperature is: room temperature-100 ℃, and extraction time is 2-12 hour, after lixiviate finishes, carry out coarse filtration, remove granule foreign, cross 400 purpose screen clothes then, further remove impurity;
D, the classification ultrafiltration is the hyperfiltration membrane assembly of 10-20 ten thousand with molecular cut off earlier, under 5-10bar pressure, above-mentioned coarse filtration liquid is carried out the ultrafiltration first time, removes macromole impurity, makes the solution clear;
To above-mentioned ultrafiltrate, the reuse molecular cut off is that 10,000 hyperfiltration membrane assembly carries out ultrafiltration, further removes impurity, collects filtrate;
To above-mentioned ultrafiltrate reuse molecular cut off is that 4000 hyperfiltration membrane assembly carries out ultrafiltration, further removes the bigger impurity of molecular weight, collects filtrate for later use;
At last, be 500 hyperfiltration membrane assembly with molecular cut off, under 35-45bar pressure, the ultrafiltrate of previous step is carried out ultrafiltration again, discard filtrate, collecting molecular weight is the ultrafiltration component of 500-4000;
E, vacuum concentration, with the molecular weight the collected ultrafiltrate in the 500-4000 component, under absolute pressure 100-200Pa, temperature is controlled to be 20-70 ℃, carries out vacuum concentration, makes its volume-diminished be the 1/5-1/10 before concentrating;
F, drying is carried out drying with concentrated solution, the brown powdery solid thing of acquisition;
G, the finished product packing storage.
The preparation method of a kind of novel anti rhzomorph preparation of the present invention, its described drying process step can adopt any one in lyophilization, the hig h-speed centrifugal spray drying; Lyophilization is that concentrated solution was carried out under-50 ℃ to-30 ℃ freezing 2-10 hour, or with liquid nitrogen flash freezer to below-30 ℃, be under the 5-10Pa in absolute pressure, carried out vacuum lyophilization 1-6 hour; Hig h-speed centrifugal spray drying is that concentrated solution is carried out centrifugal spray drying under 40000rpm, and when dry, inlet temperature is controlled at 100-110 ℃, and leaving air temp is controlled at 40-50 ℃.
The preparation method of a kind of novel anti rhzomorph preparation of the present invention, the concentration of the ethanol water that its described extracting technology step is used is 20-30%v/v.
The preparation method of a kind of novel anti rhzomorph preparation of the present invention, the leaf of the vegetable hair Cortex Populi dividianae in the pretreating process step of its described raw material is the annual leaf afterwards in May that grows to, and can be the fallen leaves in bright leaf, cured leaf, autumn.
Compared with the prior art a kind of novel anti rhzomorph preparation of the present invention has following outstanding substantive distinguishing features and marked improvement, 1, tiring of antibiotic preparation of the present invention is 1,500,000 IU/g, the limited good therapeutical effect of infection that staphylococcus, sarcina, encephalitis diplococcus etc. are caused, can replace penicillin etc., kill penicillin is produced chemical sproof pathogenic bacterium; 2, raw material resources are abundant; 3, cost is low, and production method is simple.
(4) specific embodiment:
In order to understand better and to implement, describe a kind of novel anti rhzomorph of the present invention preparation and preparation method thereof in detail below in conjunction with embodiment.
Embodiment 1, the leaf that harvesting grows to the vegetable hair Cortex Populi dividianae after May is pulverized after cleaning and drying, smashing fineness is 30 orders, ethanol water with 20%, soak the raw material of pulverizing, raw material with the water ratio is: the Cortex Populi Tomentosae raw material: water is 1: 3, extraction temperature is: 100 ℃, extraction time is 2 hours, after lixiviate finishes, carry out coarse filtration, remove granule foreign, cross 400 purpose screen clothes then, further remove impurity, then carrying out the classification ultrafiltration, is earlier 100,000 hyperfiltration membrane assembly with molecular cut off, under 5bar pressure, above-mentioned coarse filtration liquid is carried out the ultrafiltration first time, remove macromole impurity, the reuse molecular cut off is that 10,000 hyperfiltration membrane assembly carries out ultrafiltration, further removes impurity, collect filtrate, the reuse molecular cut off is that 4000 hyperfiltration membrane assembly carries out ultrafiltration, further removes the bigger impurity of molecular weight, collects filtrate for later use, at last, with molecular cut off is 500 hyperfiltration membrane assembly, under 35bar pressure, the ultrafiltrate of previous step is carried out ultrafiltration again, discard filtrate, collecting molecular weight is the ultrafiltration component of 500-4000, and under absolute pressure 100Pa, temperature is controlled to be 70 ℃, carry out vacuum concentration, make its volume-diminished be 1/5 before concentrating, with concentrated solution with liquid nitrogen flash freezer to below-30 ℃, be under the 5Pa in absolute pressure, carried out vacuum lyophilization 6 hours, the brown powdery solid thing that obtains is a kind of novel anti rhzomorph preparation of the present invention, carries out the finished product packing storage at last.
Embodiment 2, harvesting grows to the leaf of the vegetable hair Cortex Populi dividianae after May, branch and bark are pulverized after cleaning and drying, smashing fineness is 10 orders, ethanol water with 30%, soak the raw material of pulverizing, raw material with the water ratio is: the Cortex Populi Tomentosae raw material: water is 1: 7, extraction temperature is: room temperature, extraction time is 12 hours, after lixiviate finishes, carry out coarse filtration, remove granule foreign, cross 400 purpose screen clothes then, further remove impurity, then carrying out the classification ultrafiltration, is earlier 200,000 hyperfiltration membrane assembly with molecular cut off, under 10bar pressure, above-mentioned coarse filtration liquid is carried out the ultrafiltration first time, remove macromole impurity, the reuse molecular cut off is that 10,000 hyperfiltration membrane assembly carries out ultrafiltration, further removes impurity, collect filtrate, the reuse molecular cut off is that 4000 hyperfiltration membrane assembly carries out ultrafiltration, further removes the bigger impurity of molecular weight, collects filtrate for later use, at last, with molecular cut off is 500 hyperfiltration membrane assembly, under 45bar pressure, the ultrafiltrate of previous step is carried out ultrafiltration again, discard filtrate, collecting molecular weight is the ultrafiltration component of 500-4000, and under absolute pressure 200Pa, temperature is controlled to be 20 ℃, carry out vacuum concentration, making its volume-diminished for 1/10 before concentrating, concentrated solution was carried out under-30 ℃ freezing 10 hours, is under the 10Pa in absolute pressure, carried out vacuum lyophilization 1 hour, the brown powdery solid thing that obtains is a kind of novel anti rhzomorph preparation of the present invention, carries out the finished product packing storage at last.
Embodiment 3, the leaf that harvesting grows to the vegetable hair Cortex Populi dividianae after May is pulverized after cleaning and drying, smashing fineness is 20 orders, ethanol water with 95%, soak the raw material of pulverizing, raw material with the water ratio is: the Cortex Populi Tomentosae raw material: water is 1: 5, extraction temperature is: 50 ℃, extraction time is 6 hours, after lixiviate finishes, carry out coarse filtration, remove granule foreign, cross 400 purpose screen clothes then, further removing impurity, then carry out the classification ultrafiltration, is earlier 150,000 hyperfiltration membrane assembly with molecular cut off, under 8bar pressure, above-mentioned coarse filtration liquid is carried out the ultrafiltration first time, remove macromole impurity, the reuse molecular cut off is that 10,000 hyperfiltration membrane assembly carries out ultrafiltration, further remove impurity, collect filtrate, the reuse molecular cut off is that 4000 hyperfiltration membrane assembly carries out ultrafiltration, further removes the bigger impurity of molecular weight, collect filtrate for later use, at last, be 500 hyperfiltration membrane assembly with molecular cut off, under 40bar pressure, ultrafiltrate to previous step carries out ultrafiltration again, discard filtrate, collecting molecular weight is the ultrafiltration component of 500-4000, under absolute pressure 150Pa, temperature is controlled to be 45 ℃, carry out vacuum concentration, make its volume-diminished, concentrated solution is carried out centrifugal spray drying under 40000rpm for 1/8 before concentrating, when dry, inlet temperature is controlled at 100 ℃, and leaving air temp is controlled at 40 ℃, the brown powdery solid thing of acquisition, be a kind of novel anti rhzomorph preparation of the present invention, carry out the finished product packing storage at last.
Embodiment 4, winning the branch of vegetable hair Cortex Populi dividianae and bark cleans and pulverizes after drying, smashing fineness is 15 orders, ethanol water with 0%, soak the raw material of pulverizing, raw material with the water ratio is: the Cortex Populi Tomentosae raw material: water is 1: 4, extraction temperature is: 70 ℃, extraction time is 8 hours, after lixiviate finishes, carry out coarse filtration, remove granule foreign, cross 400 purpose screen clothes then, further removing impurity, then carry out the classification ultrafiltration, is earlier 160,000 hyperfiltration membrane assembly with molecular cut off, under 7bar pressure, above-mentioned coarse filtration liquid is carried out the ultrafiltration first time, remove macromole impurity, the reuse molecular cut off is that 10,000 hyperfiltration membrane assembly carries out ultrafiltration, further remove impurity, collect filtrate, the reuse molecular cut off is that 4000 hyperfiltration membrane assembly carries out ultrafiltration, further removes the bigger impurity of molecular weight, collect filtrate for later use, at last, be 500 hyperfiltration membrane assembly with molecular cut off, under 38bar pressure, ultrafiltrate to previous step carries out ultrafiltration again, discard filtrate, collecting molecular weight is the ultrafiltration component of 500-4000, under absolute pressure 120Pa, temperature is controlled to be 50 ℃, carry out vacuum concentration, make its volume-diminished, concentrated solution is carried out centrifugal spray drying under 40000rpm for 1/6 before concentrating, when dry, inlet temperature is controlled at 110 ℃, and leaving air temp is controlled at 50 ℃, the brown powdery solid thing of acquisition, be a kind of novel anti rhzomorph preparation of the present invention, carry out the finished product packing storage at last.

Claims (10)

1, a kind of novel anti rhzomorph preparation, it be by the vegetable hair Cortex Populi dividianae through pretreatment of raw material, pulverizing, lixiviate, classification ultrafiltration, vacuum concentration, drying, make finished product.
2, by the described a kind of novel anti rhzomorph preparation of claim 1, it is characterized in that described antibiotic preparation active ingredient molecular weight is 500-4000.
3,, it is characterized in that water content<5% of described antibiotic preparation by claim 1 or 2 described a kind of novel anti rhzomorph preparations.
4, the preparation method of described any one novel anti rhzomorph preparation of claim 1-3 comprises following processing step:
A, the pretreatment of raw material, the leaf of the Chinese white poplar bark of plucking a plant, branch, bark are cleaned and are dried the back as raw material;
B pulverizes, and above-mentioned raw materials is pulverized, and smashing fineness is the 10-30 order;
C, lixiviate with the ethanol water of 0-95%, is soaked the raw material of pulverizing, raw material with the water ratio is: the Cortex Populi Tomentosae raw material: water is 1: 3-7, extraction temperature is: room temperature-100 ℃, and extraction time is 2-12 hour, after lixiviate finishes, carry out coarse filtration, remove granule foreign, cross 400 purpose screen clothes then, further remove impurity;
D, the classification ultrafiltration is the hyperfiltration membrane assembly of 10-20 ten thousand with molecular cut off earlier, under 5-10bar pressure, above-mentioned coarse filtration liquid is carried out the ultrafiltration first time, removes macromole impurity;
To above-mentioned ultrafiltrate, the reuse molecular cut off is that 10,000 hyperfiltration membrane assembly carries out ultrafiltration, further removes impurity, collects filtrate;
To above-mentioned ultrafiltrate reuse molecular cut off is that 4000 hyperfiltration membrane assembly carries out ultrafiltration, further removes the bigger impurity of molecular weight, collects filtrate for later use;
At last, be 500 hyperfiltration membrane assembly with molecular cut off, under 35-45bar pressure, the ultrafiltrate of previous step is carried out ultrafiltration again, discard filtrate, collecting molecular weight is the ultrafiltration component of 500-4000;
E, vacuum concentration, with the molecular weight the collected ultrafiltrate in the 500-4000 component, under absolute pressure 100-200Pa, temperature is controlled to be 20-70 ℃, carries out vacuum concentration, makes its volume-diminished be the 1/5-1/10 before concentrating;
F, drying is carried out drying with concentrated solution, the brown powdery solid thing of acquisition;
G, the packing storage.
5, by the preparation method of the described a kind of novel anti rhzomorph preparation of claim 4, it is characterized in that described drying process step can adopt any one in lyophilization, the hig h-speed centrifugal spray drying.
6, press the preparation method of the described a kind of novel anti rhzomorph preparation of claim 5, it is characterized in that described lyophilization is that concentrated solution was carried out freezing 2-10 hour under-50 ℃ to-30 ℃, in absolute pressure is under the 5-10Pa, carries out vacuum lyophilization 1-6 hour.
7, by the preparation method of the described a kind of novel anti rhzomorph preparation of claim 5, it is characterized in that described lyophilization be with concentrated solution with liquid nitrogen flash freezer to below-30 ℃, be under the 5-10Pa in absolute pressure, carried out vacuum lyophilization 1-6 hour.
8, press the preparation method of the described a kind of novel anti rhzomorph preparation of claim 5, it is characterized in that described hig h-speed centrifugal spray drying, is that concentrated solution is carried out centrifugal spray drying under 40000rpm, when dry, inlet temperature is controlled at 100-110 ℃, and leaving air temp is controlled at 40-50 ℃.
9, by the preparation method of the described a kind of novel anti rhzomorph preparation of claim 4, it is characterized in that in the described extracting technology step, the concentration of ethanol water is 20-30%v/v.
10, press the preparation method of the described a kind of novel anti rhzomorph preparation of claim 4, the leaf that it is characterized in that the vegetable hair Cortex Populi dividianae in the pretreating process step of described raw material is the annual leaf that grows to after May, can be the fallen leaves in bright leaf, cured leaf, autumn.
CN 03112373 2003-04-30 2003-04-30 Novel antibiotic preparation and process for preparing the same Pending CN1449789A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103314007A (en) * 2010-06-02 2013-09-18 普罗马公司 Methods and strains for the production of sarcinaxanthin and derivatives thereof
CN108997457A (en) * 2018-07-10 2018-12-14 宁夏医科大学 Galuteolin and Quercetin -3-o- β-glucopyranoside extracting method in Chinese white poplar leaf

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103314007A (en) * 2010-06-02 2013-09-18 普罗马公司 Methods and strains for the production of sarcinaxanthin and derivatives thereof
CN108997457A (en) * 2018-07-10 2018-12-14 宁夏医科大学 Galuteolin and Quercetin -3-o- β-glucopyranoside extracting method in Chinese white poplar leaf
CN108997457B (en) * 2018-07-10 2022-03-08 宁夏医科大学 Method for extracting luteolin and quercetin-3-o-beta-glucopyranoside from populus tomentosa leaves

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