CN114272280B - Extraction method of safflower oil and Xinnaoqing soft capsule - Google Patents
Extraction method of safflower oil and Xinnaoqing soft capsule Download PDFInfo
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Abstract
The invention provides an extraction method of safflower oil and a Xinnaoqing soft capsule, belonging to the technical field of medicament preparation, wherein the extraction method comprises the steps of adding safflower medicinal materials and alkaline cellulase into a PBS solution, carrying out enzymolysis reaction, and then centrifuging and collecting oil bodies to obtain the safflower oil; the raw materials of the Xinnaoqing soft capsule comprise safflower oil extracted and borneol, vitamin E and vitamin B 6 . The invention utilizes alkaline cellulase to hydrolyze and break the cell wall of the safflower, so that the safflower oil is separated from the safflower cell and dispersed in water, cations in a solvent PBS solution can be immediately combined with negatively charged protein on the surface of the safflower oil separated from the safflower cell, the negative charges on the surface of the safflower oil are reduced and further aggregated into clusters, and meanwhile, the PBS solution can also inhibit the safflower oil from being oxidized.
Description
Technical Field
The invention relates to an extraction method of traditional Chinese medicinal materials, in particular to an extraction method of safflower oil and a Xinnaoqing soft capsule.
Background
The XINNAOQING Soft Capsule has effects of promoting blood circulation, removing blood stasis, dredging channels, relieving pain, inducing resuscitation and refreshing mind, and can be used for treating apoplexy, apoplexy involving the channels and collaterals, hemiplegia, facial distortion, thoracic obstruction, cardiodynia caused by blood stasis, and for treating cerebral infarction, coronary atherosclerotic heart disease, angina pectoris and hyperlipidemia.
The main raw material for preparing the Xinnaoqing soft capsule is safflower oil which is extracted from safflower.
The Carthami flos is dried flower of Carthamus tinctorius L. The safflower oil is extracted mainly by steam distillation, squeezing, solvent extraction, supercritical extraction and the like at present. However, the steam distillation method has high temperature and long time consumption, and can cause the oxidation of safflower oil; the oil yield is low by a squeezing method; solvent extraction method is easy to have solvent residue, which affects the quality of safflower oil; the equipment required for supercritical extraction is large and expensive.
In addition, the Chinese patent publication No. CN102732372B also discloses a water-phase enzyme extraction method of safflower seed oil, which adopts the crushed safflower seed kernel, takes water as a solvent, firstly carries out enzymolysis by neutral protease, then carries out enzymolysis by alkaline protease, then carries out centrifugation, demulsification by composite plant protease and secondary centrifugation, and finally obtains the safflower seed oil, the operation of the method is complex, and the moisture content of the obtained safflower oil body is high;
chinese patent publication No. CN107384582B discloses a method for extracting safflower oil, which comprises washing safflower seeds with water, soaking the seeds in PBS buffer solution, grinding the soaked seeds and PBS buffer solution with a colloid mill, centrifuging, adding sodium chloride solution, refining, layering, mixing the obtained oil body fluid with PBS emulsifier, standing, extracting oil body, and centrifuging to obtain safflower oil.
Disclosure of Invention
Aiming at the problems, the invention provides an extraction method of safflower oil and a Xinnaoqing soft capsule.
In order to realize the purpose, the technical scheme adopted by the invention is as follows:
a method for extracting safflower oil comprises adding Carthami flos (generally pulverized Carthami flos seed) and alkaline cellulase into PBS solution, performing enzymolysis reaction, centrifuging, and collecting oil body to obtain the safflower oil.
Further, the pH value of the PBS solution is 7.4-7.6.
Further, the weight ratio of the safflower medicinal material to the PBS solution is 1kg:10 to 15L.
Further, the PBS solution was prepared by taking 8 parts by weight of NaCl, 0.2 parts by weight of KCl, and 0.24 parts by weight KH 2 PO 4 And 3.63 parts by weight of Na 2 HPO 4 ·12H 2 O/1.44 parts by weight of Na 2 HPO 4 (Here, 3.63 parts by weight of Na is used 2 HPO 4 ·12H 2 O or using 1.44 parts by weight of Na 2 HPO 4 ) Adding the mixture into water of sufficient quantity to dissolve the mixture, then adjusting the pH value to 7.4-7.6, and fixing the volume to 1 part by volume to obtain the product;
the proportion of the parts by weight to the parts by volume is g: and L is used.
Further, the temperature of the enzymolysis reaction is 35-40 ℃ (preferably 36 ℃), and the time is 1-2 h.
Further, the weight ratio of the safflower medicinal material to the alkaline cellulase is 1:0.001 to 0.002.
Furthermore, the safflower medicine is also needed to be crushed before being added into the PBS solution.
Further, after being crushed, the safflower medicinal material also needs to be sieved by a sieve of 20 to 30 meshes.
The soft capsule for clearing away the heart-fire and the brain-fire comprises the following raw materials of effective components in parts by weight: 390 parts of safflower oil, 3 parts of borneol, 17 parts of vitamin E and 5 parts of vitamin B extracted by the extraction method.
Further, the preparation method of the Xinnaoqing soft capsule comprises the steps of uniformly mixing all the raw materials, and shaping, washing and drying the obtained soft capsule to obtain the Xinnaoqing soft capsule.
The extraction method of safflower oil and the Xinnaoqing soft capsule have the beneficial effects that:
the invention utilizes alkaline cellulase to hydrolyze and break the cell wall of the safflower, so that the safflower oil is separated out from the safflower cell and dispersed into water, cations in a solvent PBS solution can be immediately combined with negatively charged protein on the surface of the safflower oil separated out from the safflower cell, so that the negative charges on the surface of the safflower oil are reduced and further aggregated into clusters, and meanwhile, the PBS solution can also inhibit the safflower oil from being oxidized;
the PBS solution is used as a solvent, so that the emulsification phenomenon in the extraction process of the safflower oil can be inhibited, and the safflower oil can be directly obtained by separation without demulsification;
when the pH value of the PBS solution is 7.4-7.6, the stability of the body potential of the safflower oil can be ensured, so that the extraction rate of the safflower oil is increased, and the moisture content of the obtained safflower oil is reduced;
the extraction process of the safflower oil is simple and is easy for industrial production; the obtained safflower oil has uniform and stable oil body and good quality.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Example 1A method for extracting safflower oil
This example is a method for extracting safflower oil, the specific preparation process includes the following steps:
pulverizing Carthami flos seed, and sieving with 30 mesh sieve to obtain pulverized Carthami flos (oil content 25.0%).
Collecting 1.6kg NaCl, 40g KCl and 48g KH 2 PO 4 And 726g of Na 2 HPO 4 ·12H 2 And O, adding the solution into 150L of water, stirring and dissolving (only enough water for dissolving the raw materials such as sodium chloride is needed here, and 180L or 100L is needed), adjusting the pH value to 7.5 by using a small amount of 10wt% hydrochloric acid, and fixing the volume to 200L to prepare the PBS solution.
Taking 10kg of crushed safflower medicinal material, adding the crushed safflower medicinal material into 100L of PBS solution, stirring, adding 15g of alkaline cellulase, heating to 36 ℃, maintaining the temperature at 36 ℃ and stirring for carrying out enzymolysis reaction for 1h, after the enzymolysis reaction is finished, centrifuging at 4000r/min for 10min for water-oil separation, and collecting oil bodies, namely 1.98kg of safflower oil (marked as M1), wherein the oil body yield is 19.8 percent (the recovery rate is 79.2 percent), and the water content is 1.2 percent (the detection method of the embodiment 2 in the invention patent application with the application number of 201010562133.X is adopted for detecting the safflower oil).
The safflower oil M1 thus obtained contained 5.9% of eucalyptol, 19.7% of pilocarpus ananatide, 16.7% of lupinene- (V1), 5.3% of eicosanoic acid, 4.6% of squalene, 9.2% of methyl arachidonic acid, 4.9% of linolenic acid monoglyceride, 4.5% of 7, 10-methyl linoleate, etc.
Examples 2 to 6 extraction method of safflower oil
Examples 2 to 6 are processes for extracting safflower oil, respectively, which are substantially the same as those of example 1 except for the amount of raw materials and process parameters, and are described in detail in Table 1:
TABLE 1 summary of the process parameters of examples 2 to 6
The process parameters and procedures in the other parts of examples 2 to 6 were the same as those in example 1.
Example 7A method for preparing Xinnaoqing Soft capsules
The embodiment is a preparation method of a Xinnaoqing soft capsule, and the specific preparation process comprises the following steps of:
taking 390g of safflower oil M prepared in the example 1, adding 3g of borneol, 17g of vitamin E and 5g of vitamin B, uniformly grinding, uniformly stirring, sieving by a 100-mesh sieve, pressing into soft capsules, and then shaping, washing and drying to obtain the Xinnaoqing soft capsules, wherein the label is N1.
EXAMPLE 8-12 preparation of Xinnaoqing Soft capsules
Examples 8 to 12 are processes for preparing cardio-cerebral-vascular disease soft capsules, respectively, which are substantially the same as in example 7 except that safflower oil is used:
in example 8, safflower oil M2 purified in example 2 was used, and the obtained soft capsule for heart and brain was designated as N2;
in example 9, safflower oil M3 purified in example 3 was used, and the obtained soft capsule for cardio-cerebral vascular diseases was designated as N3;
in example 10, safflower oil M4 purified in example 4 was used, and the obtained soft capsule for cardio-cerebral-clearance was designated as N4;
in example 11, safflower oil M5 purified in example 5 was used, and the obtained soft capsule for cardio-cerebral vascular diseases was designated as N5;
in example 12, safflower oil M6 purified in example 6 was used, and the obtained soft capsule for heart and brain was designated as N6.
Experimental example 1 extraction method of safflower oil
Comparative example 1 safflower oil was extracted according to the method disclosed in the patent publication No. CN102732372B, and the obtained safflower oil was identified as DM1, and the recovery rate was 70.1%, the water content was 4.3%, the content of eucalyptol containing spoon leaves was 5.3%, the content of pilocarpine aldehyde was 17.4%, the content of lupinene- (V1) was 16.1%, the content of eicosanoic acid was 4.2%, the content of squalene was 4.5%, the content of methyl arachidonic acid was 1.2%, the content of linolenic acid monoglyceride was 1.9%, the content of 7,10-methyl linoleate was 0.7%, and the like.
Comparative example 2 according to the method disclosed in the invention patent publication No. CN107384582B, safflower oil was taken and obtained, and the safflower oil was labeled DM2, and the recovery rate was 40.1%, the water content was 3.2%, the content of eucalyptol containing spoon leaves was 5.4%, the content of pilocarpine was 17.6%, the content of lupulin- (V1) was 13.7%, the content of eicosanoic acid was 3.1%, the content of squalene was 4.6%, the content of methyl arachidonic acid was 0.1%, the content of linolenic acid monoglyceride was 0.3%, the content of 7,10-methyl linoleate was 0%, and the like.
Comparative examples 3 to 4 are comparative experiments of the extraction method of safflower oil in example 1, differing only in that:
in comparative example 3, the pH was adjusted to 6.5, and the safflower oil thus obtained was designated DM3, and the recovery rate was 69.8%, the water content was 3.4%, the content of keyhole limpet oil enol was 5.4%, lactarica villosa aldehyde was 18.6%, lupinene- (V1) was 16.3%, eicosanoic acid was 4.7%, squalene was 4.1%, methyl arachidonic acid was 7.2%, linolenic acid monoglyceride was 3.8%, 7, 10-linoleic acid methyl ester was 4.1%, etc.
In comparative example 4, the pH was adjusted to 8.5, and the safflower oil thus obtained was labeled DM4, and the recovery rate was 71.3%, the water content was 2.7%, the content of eucalyptol containing spoon leaves was 5.5%, lactonic acid was 18.2%, lupinene- (V1) was 16.5%, eicosanoic acid was 4.1%, squalene was 3.9%, methyl arachidonic acid was 8.9%, linolenic acid monoglyceride was 4.3%, 7, 10-methyl linoleate was 4.4%, and the like.
Experimental example 2 measurement of curative Effect of Xinnaoqing Soft capsules
Comparative examples 5 to 8 are comparative tests of the preparation process of the heart brain-clearing soft capsule in example 7, the differences being only that:
in the comparative example 5, safflower oil DM1 is used as a raw material, and the obtained Xinnaoqing soft capsule is marked as DN1;
in the comparative example 6, safflower oil DM2 is used as a raw material, and the obtained Xinnaoqing soft capsule is marked as DN2;
in the comparative example 7, safflower oil DM3 is used as a raw material, and the obtained Xinnaoqing soft capsule is marked as DN3;
in comparative example 8, safflower oil DM4 was used as the starting material, and the resulting Xinnaoqing soft capsule was identified as DN4.
The soft capsules of Xinnaoqing, N1-N6 and DN 1-DN 4 prepared in examples 7-12 and comparative examples 5-8 and the commercially available soft capsules of Xinnaoqing, were compared for therapeutic effect, as follows:
a1 Comparison of the effects on hypertension
Taking male SD rats weighing 250-350 g as test animals, measuring the basal blood pressure (systolic pressure) of the test animals for 3d continuously, injecting 10% chloral hydrate solution (350 mg/kg) into the abdomen of the rats on the 4 th day for anesthesia, opening the abdominal cavity, finding the right renal artery, clamping the renal artery by a silver clip with a slit of 0.2mm, closing the abdominal cavity, measuring the blood pressure of the tail artery of the rat by a sphygmomanometer after 1 week, measuring for 4 weeks continuously after 1 week, and enabling the blood pressure of the animals to reach (145 +/-12.5) mmHg. The test animals are divided into 12 groups according to blood pressure, each group comprises 10 animals, wherein a blank control group does not take any medicine, a positive control group takes the heart and brain clearing soft capsules sold in market, 1 to 6 groups respectively take the heart and brain clearing soft capsules N1 to N6 prepared in examples 7 to 12, 7 to 10 groups respectively take the heart and brain clearing soft capsules DN1 to DN4 prepared in comparative examples 5 to 8, the animals are all administrated by stomach filling, and the dosages are all 0.62g/kg. Blood pressure was measured 1 time 2h after administration, and 1 time daily for 2 weeks thereafter. Blood pressure was measured at 1 and 2 weeks after administration. And calculating the blood pressure change rate.
Blood pressure change rate (%) = (blood pressure after administration before blood pressure administration)/blood pressure before administration × 100%
The specific results are shown in the following table:
TABLE 2 summary of blood pressure changes
From table 2, it can be seen that, in the experiment of the effect on the renal artery ligation hypertension rat, the blood pressure lowering effect of the Xinnaoqing soft capsule prepared by the invention is obviously superior to that of the common Xinnaoqing soft capsule and the Xinnaoqing soft capsules DN 1-DN 4.
It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Claims (5)
1. A method for extracting safflower oil is characterized in that the method comprises the steps of adding safflower medicinal materials and alkaline cellulose into a PBS solution, carrying out enzymolysis reaction, and centrifuging to collect oil bodies to obtain the safflower oil; the pH value of the PBS solution is 7.4-7.6;
wherein the weight-volume ratio of the safflower medicinal material to the PBS solution is 1kg: 10-15L;
the PBS solution is prepared from 8 weight parts of NaCl, 0.2 weight parts of KCl and 0.24 weight parts of KH 2 PO 4 And 3.63 parts by weight of Na 2 HPO 4 ·12H 2 O/1.44 parts by weight of Na 2 HPO 4 To a sufficient amountDissolving in water, adjusting the pH value to 7.4-7.6, and fixing the volume to 1 part by volume to obtain the product; the proportion of the parts by weight to the parts by volume is g: l;
the temperature of the enzymolysis reaction is 35 to 40 ℃ and the time is 1 to 2 hours;
the weight ratio of the safflower medicinal material to the alkaline cellulase is 1:0.001 to 0.002.
2. The method for extracting safflower oil according to claim 1, wherein said safflower material is pulverized before being added to the PBS solution.
3. The method of claim 2, wherein the safflower oil is further sieved with 20-30 mesh sieve after pulverizing.
4. The Xinnaoqing soft capsule is characterized by being prepared from the following raw materials of effective components in parts by weight: 390 parts of safflower oil, 3 parts of borneol, 17 parts of vitamin E and vitamin B extracted by the extraction method of any one of claims 1 to 3 6 5 parts of the raw materials.
5. The Xinnaoqing soft capsule according to claim 4, which is prepared by uniformly mixing all the raw materials, and shaping, washing and drying the obtained soft capsule.
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| CN202111682347.5A CN114272280B (en) | 2021-12-30 | 2021-12-30 | Extraction method of safflower oil and Xinnaoqing soft capsule |
| PCT/CN2022/130319 WO2023124545A1 (en) | 2021-12-30 | 2022-11-07 | Extraction method for safflower oil and xinnaoqing soft capsule |
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| CN116421642A (en) * | 2023-03-01 | 2023-07-14 | 神威药业集团有限公司 | Xinnaoqing preparation and its preparing process |
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| JP4330312B2 (en) * | 2002-07-10 | 2009-09-16 | 昭和産業株式会社 | Oil body and method for producing oil and fat |
| CN102106891B (en) * | 2009-12-25 | 2012-11-07 | 神威药业集团有限公司 | Cardio-cerebral refreshing sustained-release soft capsules and preparation method thereof |
| CN102475733A (en) * | 2010-11-29 | 2012-05-30 | 神威药业有限公司 | Method for preparing safflower oil |
| CN102732372B (en) * | 2012-07-16 | 2014-01-22 | 渤海大学 | Water-phase enzymolysis extracting method of safflower oil |
| CN102952627B (en) * | 2012-11-22 | 2014-06-04 | 丽江坤源食品有限公司 | Method for extracting prickly ash seed oil |
| CN103919829A (en) * | 2014-03-14 | 2014-07-16 | 吉木萨尔县北庭有机食品科技有限公司 | High-oleic safflower oil soft capsule |
| CN105255577A (en) * | 2015-09-06 | 2016-01-20 | 中国林业科学研究院林产化学工业研究所 | Method for high-efficiency extraction of olive oil by utilization of aqueous enzymatic method |
| CN107384582B (en) * | 2017-09-06 | 2020-10-09 | 吉林农业大学 | Method for extracting safflower oil body |
| CN114272280B (en) * | 2021-12-30 | 2022-11-18 | 神威药业集团有限公司 | Extraction method of safflower oil and Xinnaoqing soft capsule |
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