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CN102206181A - Method for preparing norisoboldine - Google Patents

Method for preparing norisoboldine Download PDF

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CN102206181A
CN102206181A CN2011100879922A CN201110087992A CN102206181A CN 102206181 A CN102206181 A CN 102206181A CN 2011100879922 A CN2011100879922 A CN 2011100879922A CN 201110087992 A CN201110087992 A CN 201110087992A CN 102206181 A CN102206181 A CN 102206181A
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norisoboldine
preparing
crude product
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medicinal material
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CN102206181B (en
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王峥涛
侴桂新
杨莉
贺庆
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Shanghai University of Traditional Chinese Medicine
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Shanghai University of Traditional Chinese Medicine
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Abstract

本发明公开了一种制备去甲异波尔定的方法，包括从中药材中提取去甲异波尔定粗产物和对所述粗产物进行分离纯化过程，其特征在于：采用pH区带精制逆流色谱法对所述粗产物进行分离纯化。本发明所述的方法具有操作简单，溶剂消耗少，生产成本低，工艺稳定，产品纯度高，可大于等于98％，能适用于实验室和工业化半制备和制备性生产，对研究去甲异波尔定的生物活性、药理作用及开发其医药用途具有重要价值。

The invention discloses a method for preparing norisoboldine, which comprises extracting a crude product of norisoboldine from Chinese medicinal materials and carrying out a process of separating and purifying the crude product. The crude product was separated and purified by chromatography. The method of the present invention has the advantages of simple operation, less solvent consumption, low production cost, stable process, high product purity, which can be greater than or equal to 98%. Bolding's biological activity, pharmacological action and the development of its medical use are of great value.

Description

A kind of method for preparing norisoboldine
Technical field
The present invention relates to a kind of method for preparing norisoboldine, specifically, relate to the method for the norisoboldine in refining counter current chromatography separation of a kind of pH of utilization district band and the purifying Chinese medicinal materials, belong to technical field of traditional Chinese medicines.
Background technology
Norisoboldine (Norisoboidine), its chemical structural formula is as follows:
Mainly be present in the canella, as root of three-nerved spicebush root, Folium Lauri nobilis etc., this compound content in crude drug is higher.Studies show that: norisoboldine not only has antioxidation in vitro effect (Acta Pharmaceutica Sinica 200641 (10): 956～962), also can be used for treating autoimmune disorder, as: rheumatoid arthritis, multiple sclerosis, system lupus erythematosus, multiple sclerosis, type i diabetes, psoriatic, ulcerative colitis, Sjogren syndrome, scleroderma, polymyositis, chronic active hepatitis, mixed connective tissue disease, primary biliary cirrhosis, autoimmune hemolytic anemia, Hashimoto thyroiditis, the Addisons disease, hickie, the Graves disease, myasthenia gravis, ankylosing spondylitis, the allergy osteoarthritis, allergic vasculitis, autoimmunity is bitten neutrocytopenia, idiopathic thrombocytopenic purpura, systemic lupus erythematosus, chronic atrophic gastritis, autoimmunity is sterile, endometriosis, the pasture disease, pemphigus, the plate-like wolf is fullyed recover from an illness or disease (CN200810156212.3) such as dense deposit, has significant application value clinically.
But new drug development and need purity more than or equal to 98% usually now as the norisoboldine that reference material is used, and the alkaloids composition is many in the canella such as the root of three-nerved spicebush, physico-chemical property is approaching, adopt the conventional chromatogram method to be difficult to separate preparation high purity norisoboldine, and yield is very low, is unsuitable for mass preparation.Therefore, research and develop a kind of method for preparing the high purity norisoboldine, to biological activity, the pharmacological action of research norisoboldine and develop its medicinal use and have necessity and important value.
Summary of the invention
The present invention is directed to above-mentioned existing in prior technology defective and problem, a kind of method for preparing the high purity norisoboldine is provided.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of method for preparing norisoboldine comprises and extracts the norisoboldine crude product and described crude product is carried out the separation and purification process from Chinese medicinal materials, it is characterized in that: adopt the refining counter current chromatography of pH district band that described crude product is carried out separation and purification.
The solvent system of the refining counter current chromatography of described pH district band is as follows: moving phase is water, and stationary phase is an organic phase; The volume ratio of organic phase and water is 3: 7～7: 3; Contain wash-out acid in the described moving phase, the pH value is 1～5; Contain the alkali of withing a hook at the end in the described stationary phase, the pH value is 9～14.
Described organic phase is to form in 2: 8～8: 2 by normal hexane, normal-butyl tertbutyl ether or sherwood oil and propyl carbinol by volume.
Described wash-out acid is recommended as hydrochloric acid, sulfuric acid, formic acid, acetate or trifluoroacetic acid.
Described reservation alkali is recommended as ammoniacal liquor, sodium hydroxide, potassium hydroxide or triethylamine.
Described Chinese medicinal materials is a canella, refers to root of three-nerved spicebush root and Folium Lauri nobilis especially.
The process of extracting the norisoboldine crude product from root of three-nerved spicebush medicinal material is as follows: remove sandstone and impurity, root of three-nerved spicebush pulverizing medicinal materials is become to pass through 20 mesh sieves or the diameter particle less than 3cm; Oven dry is the extraction of 0～5 mineral acid aqueous solution diacolation with pH value, and the weight of used extraction solvent is 2～20 times of medicinal material weight to be extracted; Collect percolate, regulating the pH value with alkali is 7～14; Leave standstill, filter, the throw out of collection is and extracts the norisoboldine crude product that obtains.
As preferred version, the process of extracting the norisoboldine crude product from root of three-nerved spicebush medicinal material is as follows: removing sandstone and impurity, is the small-particle of 1mm to 10mm with root of three-nerved spicebush pulverizing medicinal materials; Oven dry is the extraction of 1～4 mineral acid aqueous solution diacolation with pH value, and the weight of used extraction solvent is 5～10 times of medicinal material weight to be extracted; Collect percolate, regulating the pH value with alkali is 8～10; Leave standstill, filter, the throw out of collection is and extracts the norisoboldine crude product that obtains.
The parameter of the high-speed counter-current chromatograph that band refining counter current chromatography in described pH district is used is as follows: column temperature is 15～40 ℃, and flow velocity is 0.5～20mL/min, and rotating speed is 300～1000 rev/mins.
As preferred version, the parameter of the high-speed counter-current chromatograph that band refining counter current chromatography in described pH district is used is as follows: column temperature is 20～35 ℃, and flow velocity is 1～10mL/min, and rotating speed is 400～900 rev/mins.
Norisoboldine according to method preparation of the present invention, purity 〉=98%, can be used as reference substance uses with Different Package, also can make the said formulations of several formulations such as tablet, capsule, injection liquid, also can cooperate other medicines or composition to make preparation together uses, its shared weight percent in preparation can be 0.01～99.9%, and all the other are the medicine acceptable carrier.Described pharmaceutical dosage forms can be any pharmaceutically useful formulation, and these formulations comprise: tablet, sugar coated tablet, film coated tablet, enteric coated tablet, capsule, hard capsule, soft capsule, oral liquid, suck agent, granule, electuary, pill, powder, paste, sublimed preparation, suspensoid, pulvis, solution, injection, suppository, ointment, plaster, creme, sprays, drops, patch; The preferred oral formulation, as: capsule, tablet, oral liquid, granule, pill, powder, sublimed preparation, paste etc.Described oral dosage form can contain vehicle commonly used, such as tackiness agent, weighting agent, thinner, tablet agent, lubricant, disintegrating agent, tinting material, seasonings and wetting agent, can carry out dressing to tablet in case of necessity.Suitable weighting agent comprises Mierocrystalline cellulose, mannitol, lactose and other similar weighting agent; Suitable disintegrating agent comprises starch, polyvinylpyrrolidone and starch derivative, for example sodium starch glycollate; Suitable lubricant comprises, for example Magnesium Stearate.The acceptable wetting agent of appropriate drug comprises sodium lauryl sulphate.
Compared with prior art, method of the present invention has simple to operate, and solvent consumption is few, and production cost is low, process stabilizing, and products obtained therefrom purity height (〉=98%) is applicable to laboratory and industrialization half preparation and the production of preparation property.
Description of drawings
Fig. 1 is for extracting the HPLC collection of illustrative plates of the total alkaloids crude product that obtains from root of three-nerved spicebush medicinal material.
Fig. 2 is for separating the HPLC collection of illustrative plates of the norisoboldine that obtains from the crude product that root of three-nerved spicebush medicinal material extract obtains.
The ultraviolet absorpting spectrum of the norisoboldine that Fig. 3 prepares for embodiment 1.
Specific implementation method
The present invention is described in further detail and completely below in conjunction with embodiment, but do not limit content of the present invention.
Embodiment 1
Removing sandstone and impurity, is the small-particle of 5mm with root of three-nerved spicebush pulverizing medicinal materials; Oven dry is the extraction of 2～3 aqueous sulfuric acid diacolation with pH value, and the weight of used extraction solvent is 8 times of medicinal material weight to be extracted; Collect percolate, regulating the pH value with sodium hydroxide is 8～9.5; Leave standstill, filter, the throw out of collection is and extracts the norisoboldine crude product that obtains.
Adopt the refining counter current chromatography of pH district band that described crude product is carried out separation and purification: moving phase is water, and stationary phase is an organic phase; The volume ratio of organic phase and water is 1: 1; Contain eluent hydrochloric acid in the described moving phase, the pH value is 1～2; Contain preservative ammoniacal liquor in the described stationary phase, the pH value is 9～11; Described organic phase is to form at 1: 1 by normal hexane and propyl carbinol by volume.
After stationary phase pumped into system, inject sample, pump into the moving phase wash-out again.If half countercurrent chromatography instrument, its parameter is as follows: column temperature is 30 ℃, and flow velocity is 1.5mL/min, and rotating speed is 800 rev/mins; If the countercurrent chromatography instrument, its parameter is as follows: column temperature is 30 ℃, and flow velocity is 5mL/min, and rotating speed is 400 rev/mins.
Collection contains norisoboldine stream part, sloughs inorganic salt with fillers such as MCI, Sephadex LH-20, silica gel, concentrates, and freeze-drying promptly gets norisoboldine.
Prepared norisoboldine sample is carried out high-efficient liquid phase analysis:
Chromatographic condition: Zorbax-C18 chromatographic column (4.6mm * 250mm, 5 μ m); Adopt gradient elution, for containing the aqueous solution of 0.5% formic acid and 0.1% triethylamine, Mobile phase B is an acetonitrile to mobile phase A mutually, gradient: 0min, 5%B mutually; 0～25min, 10%B; Flow velocity is 1.0mL/min; The detection wavelength is 280nm; Column temperature is 25 ℃; Sample size is 10 μ L.
The preparation of need testing solution: it is an amount of to take by weighing sample, in volumetric flask, is diluted to scale with dissolve with methanol solution, shakes up, and makes every 1mL solution and contains the 1mg sample, promptly.
Measuring method: the accurate need testing solution of drawing, inject liquid chromatograph, measure, promptly.
The purity that analysis records the norisoboldine of present embodiment preparation is 99%.
Fig. 1 is for extracting the HPLC collection of illustrative plates of the total alkaloids crude product that obtains from root of three-nerved spicebush medicinal material; Fig. 2 is for separating the HPLC collection of illustrative plates of the norisoboldine that obtains from root of three-nerved spicebush medicinal material extract crude product; The ultraviolet absorpting spectrum of the norisoboldine that Fig. 3 prepares for present embodiment.Can be known by inference by Fig. 1 to Fig. 3: the purity of the norisoboldine that is prepared by the method for the invention is very high.
Embodiment 2
Removing sandstone and impurity, is the small-particle of 1mm with root of three-nerved spicebush pulverizing medicinal materials; Oven dry is the extraction of 3～4 aqueous hydrochloric acid diacolation with pH value, and the weight of used extraction solvent is 10 times of medicinal material weight to be extracted; Collect percolate, regulating the pH value with sodium hydroxide is 8.5～9.5; Leave standstill, filter, the throw out of collection is and extracts the norisoboldine crude product that obtains.
Adopt the refining counter current chromatography of pH district band that described crude product is carried out separation and purification: moving phase is water, and stationary phase is an organic phase; The volume ratio of organic phase and water is 1: 1; Contain eluent hydrochloric acid in the described moving phase, the pH value is 1～2; Contain the preservative triethylamine in the described stationary phase, the pH value is 11～13; Described organic phase is to form at 1: 1 by normal-butyl tertbutyl ether and propyl carbinol by volume.
After stationary phase pumped into system, inject sample, pump into the moving phase wash-out again.If half countercurrent chromatography instrument, its parameter is as follows: column temperature is 30 ℃, and flow velocity is 1.5mL/min, and rotating speed is 800 rev/mins; If the countercurrent chromatography instrument, its parameter is as follows: column temperature is 30 ℃, and flow velocity is 5mL/min, and rotating speed is 400 rev/mins.
Collection contains norisoboldine stream part, sloughs inorganic salt with fillers such as MCI, Sephadex LH-20, silica gel, concentrates, and freeze-drying promptly gets norisoboldine.
Prepared norisoboldine sample is carried out high-efficient liquid phase analysis to be learnt: the purity of the norisoboldine of present embodiment preparation is 99.5%.
Embodiment 3
Removing sandstone and impurity, is the small-particle of 10mm with root of three-nerved spicebush pulverizing medicinal materials; Oven dry is the extraction of 1～2 aqueous hydrochloric acid diacolation with pH value, and the weight of used extraction solvent is 5 times of medicinal material weight to be extracted; Collect percolate, regulating the pH value with sodium hydroxide is 8～9.5; Leave standstill, filter, the throw out of collection is and extracts the norisoboldine crude product that obtains.
Adopt the refining counter current chromatography of pH district band that described crude product is carried out separation and purification: moving phase is water, and stationary phase is an organic phase; The volume ratio of organic phase and water is 1: 1; Contain eluent formic acid in the described moving phase, the pH value is 2～4; Contain the preservative triethylamine in the described stationary phase, the pH value is 11～13; Described organic phase is to form at 1: 1 by sherwood oil and propyl carbinol by volume.
After stationary phase pumped into system, inject sample, pump into the moving phase wash-out again.If half countercurrent chromatography instrument, its parameter is as follows: column temperature is 30 ℃, and flow velocity is 2mL/min, and rotating speed is 800 rev/mins; If the countercurrent chromatography instrument, its parameter is as follows: column temperature is 30 ℃, and flow velocity is 4mL/min, and rotating speed is 400 rev/mins.
Collection contains norisoboldine stream part, sloughs inorganic salt with fillers such as MCI, Sephadex LH-20, silica gel, concentrates, and freeze-drying promptly gets norisoboldine.
Prepared norisoboldine sample is carried out high-efficient liquid phase analysis to be learnt: the purity of the norisoboldine of present embodiment preparation is 98.0%.
Embodiment 4
Removing sandstone and impurity, is the small-particle of 5mm with root of three-nerved spicebush pulverizing medicinal materials; Oven dry is the extraction of 2～3 aqueous hydrochloric acid diacolation with pH value, and the weight of used extraction solvent is 10 times of medicinal material weight to be extracted; Collect percolate, regulating the pH value with ammoniacal liquor is 8.5～9.5; Leave standstill, filter, the throw out of collection is and extracts the norisoboldine crude product that obtains.
Adopt the refining counter current chromatography of pH district band that described crude product is carried out separation and purification: moving phase is water, and stationary phase is an organic phase; The volume ratio of organic phase and water is 1: 1; Contain eluent acetate in the described moving phase, the pH value is 4～5; Contain preservative potassium hydroxide in the described stationary phase, the pH value is 13～14; Described organic phase is to form at 1: 1 by normal hexane and propyl carbinol by volume.
After stationary phase pumped into system, inject sample, pump into the moving phase wash-out again.If half countercurrent chromatography instrument, its parameter is as follows: column temperature is 30 ℃, and flow velocity is 1.5mL/min, and rotating speed is 800 rev/mins; If the countercurrent chromatography instrument, its parameter is as follows: column temperature is 30 ℃, and flow velocity is 5mL/min, and rotating speed is 400 rev/mins.
Collection contains norisoboldine stream part, sloughs inorganic salt with fillers such as MCI, Sephadex LH-20, silica gel, concentrates, and freeze-drying promptly gets norisoboldine.
Prepared norisoboldine sample is carried out high-efficient liquid phase analysis to be learnt: the purity of the norisoboldine of present embodiment preparation is 98.5%.

Claims (10)

1.一种制备去甲异波尔定的方法，包括从中药材中提取去甲异波尔定粗产物和对所述粗产物进行分离纯化过程，其特征在于：采用pH区带精制逆流色谱法对所述粗产物进行分离纯化。1. A method for preparing norisoboldine, comprising extracting norisoboldine crude product from Chinese herbal medicines and carrying out separation and purification process to said crude product, is characterized in that: adopt pH zone refining countercurrent chromatography The crude product was separated and purified. 2.根据权利要求1所述的制备去甲异波尔定的方法，其特征在于，所述的pH区带精制逆流色谱法的溶剂体系如下：流动相为水相，固定相为有机相；有机相与水相的体积比为3∶7～7∶3；所述的流动相中含有洗脱酸，pH值为1～5；所述的固定相中含有保留碱，pH值为9～14。2. the method for preparing noriboridine according to claim 1 is characterized in that, the solvent system of described pH zone refining countercurrent chromatography is as follows: mobile phase is an aqueous phase, and stationary phase is an organic phase; The volume ratio of the organic phase to the aqueous phase is 3:7 to 7:3; the mobile phase contains an eluting acid, and the pH value is 1 to 5; the stationary phase contains a retained base, and the pH value is 9 to 5. 14. 3.根据权利要求2所述的制备去甲异波尔定的方法，其特征在于：所述的有机相是由正己烷、正丁基叔丁基醚或石油醚与正丁醇按体积比为2∶8～8∶2组成。3. the method for preparing norisoboldine according to claim 2 is characterized in that: described organic phase is by volume ratio by normal hexane, n-butyl tert-butyl ether or sherwood oil and n-butanol It is composed of 2:8～8:2. 4.根据权利要求2所述的制备去甲异波尔定的方法，其特征在于：所述的洗脱酸为盐酸、硫酸、甲酸、乙酸或三氟乙酸；所述的保留碱为氨水、氢氧化钠、氢氧化钾或三乙胺。4. the method for preparing noriboridine according to claim 2 is characterized in that: described eluting acid is hydrochloric acid, sulfuric acid, formic acid, acetic acid or trifluoroacetic acid; Described retaining base is ammoniacal liquor, Sodium Hydroxide, Potassium Hydroxide, or Triethylamine. 5.根据权利要求1所述的制备去甲异波尔定的方法，其特征在于：所述的中药材为樟科植物。5. the method for preparing noriboridine according to claim 1 is characterized in that: described Chinese medicinal material is Lauraceae plant. 6.根据权利要求5所述的制备去甲异波尔定的方法，其特征在于：所述的中药材为乌药药材。6. the method for preparing noribordin according to claim 5 is characterized in that: described Chinese medicinal material is black medicinal material. 7.根据权利要求6所述的制备去甲异波尔定的方法，其特征在于，从乌药药材中提取去甲异波尔定粗产物的过程如下：去除沙石及杂质，将乌药药材粉碎成能通过20目筛或者直径小于3cm的颗粒；烘干，用pH值为0～5的矿物酸水溶液渗漉提取，所用提取溶剂的重量为待提取药材重量的2～20倍；收集渗漉液，用碱调节pH值为7～14；静置，过滤，收集的沉淀物即为提取得到的去甲异波尔定粗产物。7. the method for preparing norisoboldine according to claim 6 is characterized in that, the process of extracting norisoboldine crude product from black herb medicinal material is as follows: remove sandstone and impurity, with black medicine The medicinal materials are crushed into particles that can pass through a 20-mesh sieve or have a diameter of less than 3 cm; dry, and extract by percolation with an aqueous mineral acid solution with a pH value of 0 to 5, and the weight of the extraction solvent used is 2 to 20 times the weight of the medicinal materials to be extracted; collect The percolation solution is adjusted to a pH value of 7-14 with alkali; it is left to stand and filtered, and the collected precipitate is the crude product of norisopoldine obtained by extraction. 8.根据权利要求7所述的制备去甲异波尔定的方法，其特征在于，从乌药药材中提取去甲异波尔定粗产物的过程如下：去除沙石及杂质，将乌药药材粉碎为1mm至10mm的小颗粒；烘干，用pH值为1～4的矿物酸水溶液渗漉提取，所用提取溶剂的重量为待提取药材重量的5～10倍；收集渗漉液，用碱调节pH值为8～10；静置，过滤，收集的沉淀物即为提取得到的去甲异波尔定粗产物。8. the method for preparing norisoboldine according to claim 7 is characterized in that, the process of extracting norisoboldine crude product from black herb medicinal material is as follows: remove sandstone and impurity, with black medicine The medicinal material is crushed into small particles of 1 mm to 10 mm; dried, and extracted by percolation with a mineral acid aqueous solution with a pH value of 1 to 4, and the weight of the extraction solvent used is 5 to 10 times the weight of the medicinal material to be extracted; the percolation liquid is collected and used Alkali is used to adjust the pH value to 8-10; stand still, filter, and the collected precipitate is the crude product of norisoboldine obtained by extraction. 9.根据权利要求1所述的制备去甲异波尔定的方法，其特征在于，所述的pH区带精制逆流色谱法所用的高速逆流色谱仪的参数如下：柱温为15～40℃，流速为0.5～20mL/min，转速为300～1000转/分钟。9. The method for preparing norisoboldine according to claim 1, characterized in that, the parameters of the high-speed countercurrent chromatography used in the refined countercurrent chromatography in the pH zone are as follows: column temperature is 15～40° C. , the flow rate is 0.5-20mL/min, and the rotation speed is 300-1000 rpm. 10.根据权利要求9所述的制备去甲异波尔定的方法，其特征在于，所述的pH区带精制逆流色谱法所用的高速逆流色谱仪的参数如下：柱温为20～35℃，流速为1～10mL/min，转速为400～900转/分钟。10. The method for preparing norisoboldine according to claim 9, characterized in that, the parameters of the high-speed countercurrent chromatography used in the refined countercurrent chromatography in the pH zone are as follows: column temperature is 20～35° C. , the flow rate is 1-10mL/min, and the rotation speed is 400-900 rpm.
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CN104459003A (en) * 2014-12-16 2015-03-25 湖南汉森制药股份有限公司 Construction method of standard finger-print and characteristic spectrum of Suoquan preparation and quality detection method
CN109180584A (en) * 2018-07-25 2019-01-11 湖南农业大学 A method of separating norisoboldine from the root of three-nerved spicebush

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CN102399186A (en) * 2011-12-15 2012-04-04 成都普思生物科技有限公司 Separation and purification method of norisoboldine monomer
CN102399186B (en) * 2011-12-15 2013-09-25 成都普思生物科技有限公司 Method for separating and purifying norisoboldine monomer
CN104459003A (en) * 2014-12-16 2015-03-25 湖南汉森制药股份有限公司 Construction method of standard finger-print and characteristic spectrum of Suoquan preparation and quality detection method
CN104459003B (en) * 2014-12-16 2016-01-20 湖南汉森制药股份有限公司 The construction method of contracting spring standard preparation finger-print and characteristic spectrum and quality determining method
CN109180584A (en) * 2018-07-25 2019-01-11 湖南农业大学 A method of separating norisoboldine from the root of three-nerved spicebush

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