CN102872216A - Traditional Chinese medicine preparation containing aconitum sungpanense alkaloid - Google Patents
Traditional Chinese medicine preparation containing aconitum sungpanense alkaloid Download PDFInfo
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- CN102872216A CN102872216A CN201210371583XA CN201210371583A CN102872216A CN 102872216 A CN102872216 A CN 102872216A CN 201210371583X A CN201210371583X A CN 201210371583XA CN 201210371583 A CN201210371583 A CN 201210371583A CN 102872216 A CN102872216 A CN 102872216A
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Abstract
The invention relates to a traditional Chinese medicine preparation containing aconitum sungpanense alkaloid. The preparation is of a conventional traditional Chinese medicine preparation formulation prepared from, by weight, 0.01-40% of aconitum sungpanense alkaloid extract and 60-99.99% of pharmaceutic adjuvants by the conventional process, wherein the aconitum sungpanense alkaloid extract refers to aconitum sungpanense alkaloid extractum or aconitum sungpanense alkaloid dry extract powder. The traditional Chinese medicine preparation containing the aconitum sungpanense alkaloid is stable in quality, easy to control and applicable to clinical pain management.
Description
Technical field
The present invention relates to a kind of Chinese medicine preparation, relate in particular to a kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains.
Background technology
Aconitum Sungpanense Hand-mazz is the Ranunculaceae aconitum plant, mainly be distributed in the ground such as Gansu, Qinghai, Sichuan, Shaanxi, Ningxia, Shanxi, among the peoplely be used for the treatment of the pain that traumatic injury, rheumatism, rheumatoid arthritis etc. cause, its chemical composition mainly is multiple alkaloid, and take Diterpenoid Alkaloids as main, Diterpenoid Alkaloids is as the main effective ingredient of Aconitum Sungpanense Hand-mazz, and its pharmacologically active is mainly manifested in the aspects such as analgesia, calmness, analgesic, antiinflammatory, and without toleration and health according to patience.
Alkaloid is a class basic nitrogen compound, exist mainly with the form of salt greatly at nature, have been reported for the alkaloidal method for extraction and purification of Aconitum Sungpanense Hand-mazz at present, Chinese patent CN101037412A discloses a kind of method of extracting chasmanine from Aconitum Sungpanense Hand-mazz, and Chinese patent CN101851202A has announced the preparation method of the black first element of a kind of pine; Chinese patent CN101829201A has announced a kind of alkaloidal method of extracting from monkshood medicinal material; Above three kinds of methods all adopt classical chemical method, and extraction step is various, and complicated operation can not be suitable for large-scale production, and exists product purity not high, and production cost is high, the problems such as serious environment pollution.Therefore, people's expectation can provide a kind of simple and effective Aconitum Sungpanense Hand-mazz alkaloid method for extraction and purification.
The human puzzlement that all the time is subject to disease, in many cases, disease also causes the misery of the human body except the forfeiture that causes function of human body or even life, for example: late gastric cancer, wound etc.In order to alleviate patient's misery, people have developed many analgesics.The most effective analgesic has morphine, dolantin in the at present clinical practice.But the disadvantage of this medicine is exactly that life-time service can produce dependency and addiction.Therefore, it is a kind of imperative according to the patience analgesic without toleration and health to study, so far, do not occur take effective site as object of study, investigate the source investigation of Aconitum Sungpanense Hand-mazz alkaloid valid target comprehensively, also do not have the Chinese medicine preparation of making as active component take high-load Aconitum Sungpanense Hand-mazz alkaloid to be applied to clinical.
Summary of the invention
Technical problem to be solved by this invention provides a kind of steady quality, be easy to control, contain Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation applicable to clinical practice.
For addressing the above problem, a kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains of the present invention is characterized in that: said preparation is with the percentage by weight Chinese medicine regular dosage form preparation made of technique routinely by 0.01 ~ 40% Aconitum Sungpanense Hand-mazz alkaloid extract and 60 ~ 99.99% pharmaceutic adjuvants; Described Aconitum Sungpanense Hand-mazz alkaloid extract refers to Aconitum Sungpanense Hand-mazz alkaloid extractum or Aconitum Sungpanense Hand-mazz alkaloid dried cream powder.
Described Aconitum Sungpanense Hand-mazz alkaloid extractum is to make as follows:
⑴ add successively ammonia reagent, mass concentration in the Aconitum Sungpanense Hand-mazz medical material of rear mistake 60 mesh sieves of pulverizing be that 40% ~ 95% ethanol fully stirs, and is that 70 ℃ ~ 80 ℃, power are supersound extraction 30 ~ 60min under the condition of 500W in temperature, obtains extracting solution A; The mass volume ratio of described Aconitum Sungpanense Hand-mazz medical material and described ammonia reagent is 1:1 ~ 1:2; The mass volume ratio of described Aconitum Sungpanense Hand-mazz medical material and described ethanol is 1:10 ~ 1:40;
Described extracting solution A carries out sucking filtration under the condition of 0.07 ~ 0.09MPa, obtain filtrate, and this filtrate through being evaporated to without ethanol, namely gets alkaloid extractum under 0.06 ~ 0.08MPa; Adding acid solution in described alkaloid extractum, to transfer to pH value be 2, be that 70 ℃ ~ 80 ℃, power are supersound extraction 10 ~ 30min under the condition of 500W in temperature, obtain extracting solution B, this extracting solution B obtains supernatant C with centrifugalize under 3500 ~ 4500 rev/mins the rotating speed---the Aconitum Sungpanense Hand-mazz alkaloids extract;
⑵ described Aconitum Sungpanense Hand-mazz alkaloids extract with ammonia reagent transfer to that pH is 4 ~ 7, after concentration is 0.1 ~ 0.3g/ml, through macroporous resin adsorption 30 ~ 60min, be 50 ~ 95% ethanol elution more successively with deionized water, mass concentration, collect ethanol elution, until eluent pH value be under 2 ~ 3 the acid condition with bismuth potassium iodide, Wagner's reagent, Mayer's reagent, etc. the reaction of alkaloid precipitant stop when all being negative collecting; Described ethanol elution through decompression recycling ethanol, namely gets proportion and is 1.1 ~ 1.3 Aconitum Sungpanense Hand-mazz alkaloid extractum under 60 ℃, 0.06 ~ 0.08MPa.
Replace above-mentioned steps ⑴ to prepare the Aconitum Sungpanense Hand-mazz alkaloids extract with following preparation method: the adding pH value is 2 acid solution in the Aconitum Sungpanense Hand-mazz medical material of rear mistake 60 mesh sieves of pulverizing, be that 70 ℃ ~ 80 ℃, power are supersound extraction 60 ~ 120min under the condition of 500W in temperature, obtain extracting solution A, this extracting solution A obtains supernatant B and precipitate with centrifugalize under 3500 ~ 4500 rev/mins the rotating speed; Described precipitate pH value is 2 acid solution washed twice, obtains supernatant C; Merge supernatant B and supernatant C, namely get the Aconitum Sungpanense Hand-mazz alkaloids extract.
Replace above-mentioned steps ⑵ to prepare Aconitum Sungpanense Hand-mazz alkaloid extractum with following preparation method: described Aconitum Sungpanense Hand-mazz alkaloids extract adopts ultrafilter membrane, be that 0.06 ~ 0.08MPa, feed temperature are that 20 ~ 40 ℃, feed volume flow are to filter under the condition of 2.0 ~ 3.0L/min at pressure, obtain filtrate; Described filtrate through decompression recycling ethanol, namely gets proportion and is 1.1 ~ 1.3 Aconitum Sungpanense Hand-mazz alkaloid extractum under 60 ℃, 0.06 ~ 0.08Mpa.
Described ammonia reagent refers to that the volume ratio of ammonia and water is the solution of 2:3.
Acid solution among the described step ⑴ refers to that mass concentration is a kind of in 0.5% ~ 2% sulphuric acid, hydrochloric acid or the acetic acid.
Macroporous resin among the described step ⑵ refers to a kind of among D101, X-5 or the AB-8.
The relative molecular mass of holding back of described ultrafilter membrane is 1000 ~ 10000.
It is to be dried to constant weight under the condition of 0.06 ~ 5Pa for-60 ~ 60 ℃, pressure in temperature that described Aconitum Sungpanense Hand-mazz alkaloid dried cream powder refers to Aconitum Sungpanense Hand-mazz alkaloid extractum, through being crushed to the dried cream powder of 80 ~ 120 order gained.
The present invention compared with prior art has the following advantages:
1, the alcohol extracting method wide adaptability of the present invention's employing, water-solubility impurity is less in the alkaloid that extracts.
2, the sour lifting manipulation of the present invention's employing can increase the dissolubility of alkaloid in water, and method is easier.
3, the present invention adopts Amberlyst process, and is easy and simple to handle, and cost is lower, but and the resin Reusability, be fit to commercial production.
4, the ultra-filtration process that adopts of invention is to carry out at normal temperatures, and mild condition is destroyed without composition, is a kind of isolation technics of energy-conserving and environment-protective, and segregation apparatus is simple, flow process is short, easy and simple to handle, be easy to control and safeguard.
5, the Aconitum Sungpanense Hand-mazz alkaloid that extracts with the inventive method carries out relevant analgesia pharmacodynamic study.
5.1 hot plate method analgesic experiment
Select 50 of Kunming kind female mices, body weight 18 ~ 22g, by the body weight random packet, 10 every group.Do positive control with morphine hydrochloride, do negative control with normal saline.
Measure each experimental mouse threshold of pain with hot plate method, the medicine by requirement of experiment gives various dose for each experimental mice gavage respectively, calculate the threshold of pain with following formula and improve percentage rate:
N=(n-n
0)/n
0* 100% wherein: n
0Be pain threshold before the administration; N is pain threshold after the administration.
Table 1 hot plate method analgesic experiment result
In the table:
▲Compare with the normal saline group,
▲P ﹤ 0.05; * compare * P ﹤ 0.05 with the morphine hydrochloride group.
The result shows, Aconitum Sungpanense Hand-mazz alkaloid analgesic activity is remarkable, though onset is slow than morphine, analgesic effect is stable lasting.
5.2 acetic acid twisting method analgesic experiment
Select at random the grouping of male and female half and half experiment mice to test by acetic acid twisting method analgesic experiment method by body weight, statistics normal saline group is behind the administration 1h, behind the morphine hydrochloride group administration 0.5h, behind Aconitum Sungpanense Hand-mazz (6mg/kg) the group administration 3h, behind Aconitum Sungpanense Hand-mazz (12mg/kg) the group administration 2.5h, inject again the writhing number of times in 0.7% acetic acid 10ml/kg, the 15min, statistical procedures is carried out in grouping, calculates the writhing suppression ratio.
Table 2 acetic acid twisting method analgesic experiment result
In the table:
▲Compare with the normal saline group,
▲P ﹤ 0.05; * compare * P ﹤ 0.05 with the morphine hydrochloride group.
The result shows that Aconitum Sungpanense Hand-mazz can significantly suppress the mouse writhing reaction that acetic acid causes.
Conclusion: Aconitum Sungpanense Hand-mazz total alkaloids analgesic effect is obvious, can significantly improve the mice pain threshold.The preparation that makes with the inventive method is used for pain management, and steady quality, dosage are easy to control, applicable to clinical practice.
The specific embodiment
Embodiment 1A kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains, said preparation is by 0.01% Aconitum Sungpanense Hand-mazz alkaloid extract---Aconitum Sungpanense Hand-mazz alkaloid extractum and 99.99% pharmaceutic adjuvant are with the percentage by weight Chinese medicine regular dosage form preparation made of technique routinely.
Wherein:
Aconitum Sungpanense Hand-mazz alkaloid extractum is to make as follows:
⑴ add successively ammonia reagent, mass concentration in the Aconitum Sungpanense Hand-mazz medical material of rear mistake 60 mesh sieves of pulverizing be that 40% ethanol fully stirs, and is that 70 ℃, power are supersound extraction 60min under the condition of 500W in temperature, obtains extracting solution A; The mass volume ratio of Aconitum Sungpanense Hand-mazz medical material and ammonia reagent (kg/ml) is 1:1; The mass volume ratio of Aconitum Sungpanense Hand-mazz medical material and ethanol (kg/ml) is 1:10.
Extracting solution A carries out sucking filtration under the condition of 0.07MPa, obtain filtrate, and this filtrate through being evaporated to without ethanol, namely gets alkaloid extractum under 0.06MPa; Adding acid solution in alkaloid extractum, to transfer to pH value be 2, be that 70 ℃, power are supersound extraction 30min under the condition of 500W in temperature, obtain extracting solution B, is this extracting solution B with centrifugalize under 3500 rev/mins the rotating speed? ~? minute, obtain supernatant C---the Aconitum Sungpanense Hand-mazz alkaloids extract.
⑵ Aconitum Sungpanense Hand-mazz alkaloids extract with ammonia reagent transfer to that pH is 4 ~ 7, after concentration is 0.1 ~ 0.3g/ml, through macroporous resin adsorption 30min, be 50% ethanol elution more successively with deionized water, mass concentration, collect ethanol elution, until eluent pH value be under 2 ~ 3 the acid condition with bismuth potassium iodide, Wagner's reagent, Mayer's reagent, etc. the reaction of alkaloid precipitant stop when all being negative collecting; Ethanol elution through decompression recycling ethanol, namely gets proportion and is 1.1 ~ 1.3 Aconitum Sungpanense Hand-mazz alkaloid extractum under 60 ℃, 0.06MPa.
Embodiment 2A kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains, said preparation is by 40% Aconitum Sungpanense Hand-mazz alkaloid extract---Aconitum Sungpanense Hand-mazz alkaloid extractum and 60% pharmaceutic adjuvant are with the percentage by weight Chinese medicine regular dosage form preparation made of technique routinely.
Wherein:
Aconitum Sungpanense Hand-mazz alkaloid extractum is to make as follows:
⑴ add successively ammonia reagent, mass concentration in the Aconitum Sungpanense Hand-mazz medical material of rear mistake 60 mesh sieves of pulverizing be that 95% ethanol fully stirs, and is that 80 ℃, power are supersound extraction 30min under the condition of 500W in temperature, obtains extracting solution A; The mass volume ratio of Aconitum Sungpanense Hand-mazz medical material and ammonia reagent (kg/ml) is 1:2; The mass volume ratio of Aconitum Sungpanense Hand-mazz medical material and ethanol (kg/ml) is 1:40.
Extracting solution A carries out sucking filtration under the condition of 0.09MPa, obtain filtrate, and this filtrate through being evaporated to without ethanol, namely gets alkaloid extractum under 0.08MPa; Adding acid solution in alkaloid extractum, to transfer to pH value be 2, be that 80 ℃, power are supersound extraction 10min under the condition of 500W in temperature, obtain extracting solution B, is this extracting solution B with centrifugalize under 4500 rev/mins the rotating speed? ~? minute, obtain supernatant C---the Aconitum Sungpanense Hand-mazz alkaloids extract.
⑵ Aconitum Sungpanense Hand-mazz alkaloids extract with ammonia reagent transfer to that pH is 4 ~ 7, after concentration is 0.1 ~ 0.3g/ml, through macroporous resin adsorption 60min, be 95% ethanol elution more successively with deionized water, mass concentration, collect ethanol elution, until eluent pH value be under 2 ~ 3 the acid condition with bismuth potassium iodide, Wagner's reagent, Mayer's reagent, etc. the reaction of alkaloid precipitant stop when all being negative collecting; Ethanol elution through decompression recycling ethanol, namely gets proportion and is 1.1 ~ 1.3 Aconitum Sungpanense Hand-mazz alkaloid extractum under 60 ℃, 0.08MPa.
Embodiment 3A kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains, said preparation is by 0.1% Aconitum Sungpanense Hand-mazz alkaloid extract---Aconitum Sungpanense Hand-mazz alkaloid extractum and 99.9% pharmaceutic adjuvant are with the percentage by weight Chinese medicine regular dosage form preparation made of technique routinely.
Wherein:
Aconitum Sungpanense Hand-mazz alkaloid extractum is to make as follows:
⑴ add successively ammonia reagent, mass concentration in the Aconitum Sungpanense Hand-mazz medical material of rear mistake 60 mesh sieves of pulverizing be that 50% ethanol fully stirs, and is that 75 ℃, power are supersound extraction 45min under the condition of 500W in temperature, obtains extracting solution A; The mass volume ratio of Aconitum Sungpanense Hand-mazz medical material and ammonia reagent (kg/ml) is 1:1.5; The mass volume ratio of Aconitum Sungpanense Hand-mazz medical material and described ethanol (kg/ml) is 1:25.
Extracting solution A carries out sucking filtration under the condition of 0.08MPa, obtain filtrate, and this filtrate through being evaporated to without ethanol, namely gets alkaloid extractum under 0.07MPa; Adding acid solution in alkaloid extractum, to transfer to pH value be 2, be that 75 ℃, power are supersound extraction 20min under the condition of 500W in temperature, obtain extracting solution B, is this extracting solution B with centrifugalize under 4000 rev/mins the rotating speed? ~? minute, obtain supernatant C---the Aconitum Sungpanense Hand-mazz alkaloids extract.
⑵ Aconitum Sungpanense Hand-mazz alkaloids extract with ammonia reagent transfer to that pH is 4 ~ 7, after concentration is 0.1 ~ 0.3g/ml, through macroporous resin adsorption 45min, be 60% ethanol elution more successively with deionized water, mass concentration, collect ethanol elution, until eluent pH value be under 2 ~ 3 the acid condition with bismuth potassium iodide, Wagner's reagent, Mayer's reagent, etc. the reaction of alkaloid precipitant stop when all being negative collecting; Ethanol elution through decompression recycling ethanol, namely gets proportion and is 1.1 ~ 1.3 Aconitum Sungpanense Hand-mazz alkaloid extractum under 60 ℃, 0.07MPa.
Embodiment 4A kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains, said preparation is by 1% Aconitum Sungpanense Hand-mazz alkaloid extract---Aconitum Sungpanense Hand-mazz alkaloid extractum and 99% pharmaceutic adjuvant are with the percentage by weight Chinese medicine regular dosage form preparation made of technique routinely.
Wherein:
Aconitum Sungpanense Hand-mazz alkaloid extractum is to make as follows:
⑴ add pH value in the Aconitum Sungpanense Hand-mazz medical material of rear mistake 60 mesh sieves of pulverizing be 2 acid solution, be that 70 ℃, power are supersound extraction 60min under the condition of 500W in temperature, obtain extracting solution A, is this extracting solution A with centrifugalize under 3500 rev/mins the rotating speed? ~? minute, obtain supernatant B and precipitate; The precipitate pH value is 2 acid solution washed twice, obtains supernatant C; Merge supernatant B and supernatant C, namely get the Aconitum Sungpanense Hand-mazz alkaloids extract.
⑵ Aconitum Sungpanense Hand-mazz alkaloids extract with ammonia reagent transfer to that pH is 4 ~ 7, after concentration is 0.1 ~ 0.3g/ml, through macroporous resin adsorption 40min, be 60% ethanol elution more successively with deionized water, mass concentration, collect ethanol elution, until eluent pH value be under 2 ~ 3 the acid condition with bismuth potassium iodide, Wagner's reagent, Mayer's reagent, etc. the reaction of alkaloid precipitant stop when all being negative collecting; Ethanol elution through decompression recycling ethanol, namely gets proportion and is 1.1 ~ 1.3 Aconitum Sungpanense Hand-mazz alkaloid extractum under 60 ℃, 0.06MPa.
Embodiment 5A kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains, said preparation is by 5% Aconitum Sungpanense Hand-mazz alkaloid extract---Aconitum Sungpanense Hand-mazz alkaloid extractum and 95% pharmaceutic adjuvant are with the percentage by weight Chinese medicine regular dosage form preparation made of technique routinely.
Wherein:
Aconitum Sungpanense Hand-mazz alkaloid extractum is to make as follows:
⑴ add pH value in the Aconitum Sungpanense Hand-mazz medical material of rear mistake 60 mesh sieves of pulverizing be 2 acid solution, be that 80 ℃, power are supersound extraction 120min under the condition of 500W in temperature, obtain extracting solution A, is this extracting solution A with centrifugalize under 4500 rev/mins the rotating speed? ~? minute, obtain supernatant B and precipitate; The precipitate pH value is 2 acid solution washed twice, obtains supernatant C; Merge supernatant B and supernatant C, namely get the Aconitum Sungpanense Hand-mazz alkaloids extract.
⑵ Aconitum Sungpanense Hand-mazz alkaloids extract with ammonia reagent transfer to that pH is 4 ~ 7, after concentration is 0.1 ~ 0.3g/ml, through macroporous resin adsorption 50min, be 70% ethanol elution more successively with deionized water, mass concentration, collect ethanol elution, until eluent pH value be under 2 ~ 3 the acid condition with bismuth potassium iodide, Wagner's reagent, Mayer's reagent, etc. the reaction of alkaloid precipitant stop when all being negative collecting; Ethanol elution through decompression recycling ethanol, namely gets proportion and is 1.1 ~ 1.3 Aconitum Sungpanense Hand-mazz alkaloid extractum under 60 ℃, 0.08MPa.
Embodiment 6A kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains, said preparation is by 10% Aconitum Sungpanense Hand-mazz alkaloid extract---Aconitum Sungpanense Hand-mazz alkaloid extractum and 90% pharmaceutic adjuvant are with the percentage by weight Chinese medicine regular dosage form preparation made of technique routinely.
Wherein:
Aconitum Sungpanense Hand-mazz alkaloid extractum is to make as follows:
⑴ add pH value in the Aconitum Sungpanense Hand-mazz medical material of rear mistake 60 mesh sieves of pulverizing be 2 acid solution, be that 75 ℃, power are supersound extraction 90min under the condition of 500W in temperature, obtain extracting solution A, this extracting solution A obtains supernatant B and precipitate with centrifugalize under 4000 rev/mins the rotating speed; The precipitate pH value is 2 acid solution washed twice, obtains supernatant C; Merge supernatant B and supernatant C, namely get the Aconitum Sungpanense Hand-mazz alkaloids extract.
⑵ Aconitum Sungpanense Hand-mazz alkaloids extract with ammonia reagent transfer to that pH is 4 ~ 7, after concentration is 0.1 ~ 0.3g/ml, through macroporous resin adsorption 50min, be 80% ethanol elution more successively with deionized water, mass concentration, collect ethanol elution, until eluent pH value be under 2 ~ 3 the acid condition with bismuth potassium iodide, Wagner's reagent, Mayer's reagent, etc. the reaction of alkaloid precipitant stop when all being negative collecting; Ethanol elution through decompression recycling ethanol, namely gets proportion and is 1.1 ~ 1.3 Aconitum Sungpanense Hand-mazz alkaloid extractum under 60 ℃, 0.07MPa.
Embodiment 7A kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains, said preparation is by 20% Aconitum Sungpanense Hand-mazz alkaloid extract---Aconitum Sungpanense Hand-mazz alkaloid extractum and 80% pharmaceutic adjuvant are with the percentage by weight Chinese medicine regular dosage form preparation made of technique routinely.
Wherein:
Aconitum Sungpanense Hand-mazz alkaloid extractum is to make as follows:
⑴ same
Embodiment 1 ~ 6
⑵ Aconitum Sungpanense Hand-mazz alkaloids extract adopts and to hold back relative molecular mass is 1000 ultrafilter membrane, is that 0.06MPa, feed temperature are that 20 ℃, feed volume flow are to filter under the condition of 2.0L/min at pressure, obtains filtrate; Filtrate through decompression recycling ethanol, namely gets proportion and is 1.1 ~ 1.3 Aconitum Sungpanense Hand-mazz alkaloid extractum under 60 ℃, 0.06Mpa.
Embodiment 8A kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains, said preparation is by 30% Aconitum Sungpanense Hand-mazz alkaloid extract---Aconitum Sungpanense Hand-mazz alkaloid extractum and 70% pharmaceutic adjuvant are with the percentage by weight Chinese medicine regular dosage form preparation made of technique routinely.
Wherein:
Aconitum Sungpanense Hand-mazz alkaloid extractum is to make as follows:
⑴ same
Embodiment 1 ~ 6
⑵ Aconitum Sungpanense Hand-mazz alkaloids extract adopts and to hold back relative molecular mass is 10000 ultrafilter membrane, is that 0.08MPa, feed temperature are that 40 ℃, feed volume flow are to filter under the condition of 3.0L/min at pressure, obtains filtrate; Filtrate through decompression recycling ethanol, namely gets proportion and is 1.1 ~ 1.3 Aconitum Sungpanense Hand-mazz alkaloid extractum under 60 ℃, 0.08Mpa.
Embodiment 9A kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains, said preparation is by 15% Aconitum Sungpanense Hand-mazz alkaloid extract---Aconitum Sungpanense Hand-mazz alkaloid extractum and 85% pharmaceutic adjuvant are with the percentage by weight Chinese medicine regular dosage form preparation made of technique routinely.
Wherein:
Aconitum Sungpanense Hand-mazz alkaloid extractum is to make as follows:
⑴ same
Embodiment 1 ~ 6
⑵ Aconitum Sungpanense Hand-mazz alkaloids extract adopts and to hold back relative molecular mass is 5000 ultrafilter membrane, is that 0.07MPa, feed temperature are that 30 ℃, feed volume flow are to filter under the condition of 2.5L/min at pressure, obtains filtrate; Filtrate through decompression recycling ethanol, namely gets proportion and is 1.1 ~ 1.3 Aconitum Sungpanense Hand-mazz alkaloid extractum under 60 ℃, 0.07Mpa.
Embodiment 10A kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains, said preparation is by 25% Aconitum Sungpanense Hand-mazz alkaloid extract---Aconitum Sungpanense Hand-mazz alkaloid dried cream powder and 75% pharmaceutic adjuvant are with the percentage by weight Chinese medicine regular dosage form preparation made of technique routinely.
Wherein:
Aconitum Sungpanense Hand-mazz alkaloid dried cream powder refer to
Embodiment 1 ~ 9The Aconitum Sungpanense Hand-mazz alkaloid extractum that obtains is to be dried to constant weight under the condition of 0.06Pa for-60 ℃, pressure in temperature, through being crushed to the dried cream powder of 80 ~ 120 order gained.
Embodiment 11A kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains, said preparation is by 35% Aconitum Sungpanense Hand-mazz alkaloid extract---Aconitum Sungpanense Hand-mazz alkaloid dried cream powder and 65% pharmaceutic adjuvant are with the percentage by weight Chinese medicine regular dosage form preparation made of technique routinely.
Wherein:
Aconitum Sungpanense Hand-mazz alkaloid dried cream powder refer to
Embodiment 1 ~ 9The Aconitum Sungpanense Hand-mazz alkaloid extractum that obtains is that 60 ℃, pressure are to be dried to constant weight under the condition of 5Pa in temperature, through being crushed to the dried cream powder of 80 ~ 120 order gained.
Embodiment 12A kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains, said preparation is by 0.05% Aconitum Sungpanense Hand-mazz alkaloid extract---Aconitum Sungpanense Hand-mazz alkaloid dried cream powder and 99.95% pharmaceutic adjuvant are with the percentage by weight Chinese medicine regular dosage form preparation made of technique routinely.
Wherein:
Aconitum Sungpanense Hand-mazz alkaloid dried cream powder refer to
Embodiment 1 ~ 9The Aconitum Sungpanense Hand-mazz alkaloid extractum that obtains is that 0 ℃, pressure are to be dried to constant weight under the condition of 0.5Pa in temperature, through being crushed to the dried cream powder of 80 ~ 120 order gained.
Above-mentioned
Embodiment 1 ~ 12In, ammonia reagent refers to that the volume ratio of ammonia and water is the solution of 2:3.Acid solution among the step ⑴ refers to that mass concentration is a kind of in 0.5% ~ 2% sulphuric acid, hydrochloric acid or the acetic acid.Macroporous resin among the step ⑵ refers to a kind of among D101, X-5 or the AB-8.
Claims (9)
1. one kind contains Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation, it is characterized in that: said preparation is with the percentage by weight Chinese medicine regular dosage form preparation made of technique routinely by 0.01 ~ 40% Aconitum Sungpanense Hand-mazz alkaloid extract and 60 ~ 99.99% pharmaceutic adjuvants; Described Aconitum Sungpanense Hand-mazz alkaloid extract refers to Aconitum Sungpanense Hand-mazz alkaloid extractum or Aconitum Sungpanense Hand-mazz alkaloid dried cream powder.
2. a kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains as claimed in claim 1, it is characterized in that: described Aconitum Sungpanense Hand-mazz alkaloid extractum is to make as follows:
⑴ add successively ammonia reagent, mass concentration in the Aconitum Sungpanense Hand-mazz medical material of rear mistake 60 mesh sieves of pulverizing be that 40% ~ 95% ethanol fully stirs, and is that 70 ℃ ~ 80 ℃, power are supersound extraction 30 ~ 60min under the condition of 500W in temperature, obtains extracting solution A; The mass volume ratio of described Aconitum Sungpanense Hand-mazz medical material and described ammonia reagent is 1:1 ~ 1:2; The mass volume ratio of described Aconitum Sungpanense Hand-mazz medical material and described ethanol is 1:10 ~ 1:40;
Described extracting solution A carries out sucking filtration under the condition of 0.07 ~ 0.09MPa, obtain filtrate, and this filtrate through being evaporated to without ethanol, namely gets alkaloid extractum under 0.06 ~ 0.08MPa; Adding acid solution in described alkaloid extractum, to transfer to pH value be 2, be that 70 ℃ ~ 80 ℃, power are supersound extraction 10 ~ 30min under the condition of 500W in temperature, obtain extracting solution B, this extracting solution B obtains supernatant C with centrifugalize under 3500 ~ 4500 rev/mins the rotating speed---the Aconitum Sungpanense Hand-mazz alkaloids extract;
⑵ described Aconitum Sungpanense Hand-mazz alkaloids extract with ammonia reagent transfer to that pH is 4 ~ 7, after concentration is 0.1 ~ 0.3g/ml, through macroporous resin adsorption 30 ~ 60min, be 50 ~ 95% ethanol elution more successively with deionized water, mass concentration, collect ethanol elution, until eluent pH value be under 2 ~ 3 the acid condition with bismuth potassium iodide, Wagner's reagent, Mayer's reagent, etc. the reaction of alkaloid precipitant stop when all being negative collecting; Described ethanol elution through decompression recycling ethanol, namely gets proportion and is 1.1 ~ 1.3 Aconitum Sungpanense Hand-mazz alkaloid extractum under 60 ℃, 0.06 ~ 0.08MPa.
3. a kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains as claimed in claim 2, it is characterized in that: prepare the Aconitum Sungpanense Hand-mazz alkaloids extract with step ⑴ described in the following preparation method replacement claim 2: the adding pH value is 2 acid solution in the Aconitum Sungpanense Hand-mazz medical material of rear mistake 60 mesh sieves of pulverizing, be that 70 ℃ ~ 80 ℃, power are supersound extraction 60 ~ 120min under the condition of 500W in temperature, obtain extracting solution A, this extracting solution A obtains supernatant B and precipitate with centrifugalize under 3500 ~ 4500 rev/mins the rotating speed; Described precipitate pH value is 2 acid solution washed twice, obtains supernatant C; Merge supernatant B and supernatant C, namely get the Aconitum Sungpanense Hand-mazz alkaloids extract.
4. a kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains as claimed in claim 2, it is characterized in that: prepare Aconitum Sungpanense Hand-mazz alkaloid extractum with step ⑵ described in the following preparation method replacement claim 2: described Aconitum Sungpanense Hand-mazz alkaloids extract adopts ultrafilter membrane, be that 0.06 ~ 0.08MPa, feed temperature are that 20 ~ 40 ℃, feed volume flow are to filter under the condition of 2.0 ~ 3.0L/min at pressure, obtain filtrate; Described filtrate through decompression recycling ethanol, namely gets proportion and is 1.1 ~ 1.3 Aconitum Sungpanense Hand-mazz alkaloid extractum under 60 ℃, 0.06 ~ 0.08Mpa.
5. a kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains as claimed in claim 2, it is characterized in that: described ammonia reagent refers to that the volume ratio of ammonia and water is the solution of 2:3.
6. a kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains as claimed in claim 2 or claim 3 is characterized in that: the acid solution among the described step ⑴ refers to that mass concentration is a kind of in 0.5% ~ 2% sulphuric acid, hydrochloric acid or the acetic acid.
7. a kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains as claimed in claim 2 is characterized in that: the macroporous resin among the described step ⑵ refers to a kind of among D101, X-5 or the AB-8.
8. a kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains as claimed in claim 4, it is characterized in that: the relative molecular mass of holding back of described ultrafilter membrane is 1000 ~ 10000.
9. a kind of Aconitum Sungpanense Hand-mazz alkaloid Chinese medicine preparation that contains as claimed in claim 1, it is characterized in that: it is to be dried to constant weight under the condition of 0.06 ~ 5Pa for-60 ~ 60 ℃, pressure in temperature that described Aconitum Sungpanense Hand-mazz alkaloid dried cream powder refers to Aconitum Sungpanense Hand-mazz alkaloid extractum, through being crushed to the dried cream powder of 80 ~ 120 order gained.
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