CN115433079B - Method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation - Google Patents
Method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation Download PDFInfo
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Abstract
The application discloses a method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation, which belongs to the technical field of traditional Chinese medicine extraction and comprises the following steps: drying rhizoma Ligustici Chuanxiong, sealing in packaging bag, and storing in dark place; irradiating the packaged rhizoma Ligustici Chuanxiong at normal temperature with low dose; pulverizing the irradiated rhizoma Ligustici Chuanxiong; adding the crushed Ligusticum wallichii into the extractant, soaking in dark, carrying out ultrasonic treatment, and filtering to obtain supernatant. The extraction is carried out after the Ligusticum wallichii is irradiated, so that the extraction yield of three active substances in the Ligusticum wallichii is obviously improved.
Description
Technical Field
The application relates to the technical field of traditional Chinese medicine extraction, in particular to a method for improving the extraction efficiency of active ingredients of ligusticum wallichii by irradiation.
Background
The related research and development of Ligusticum chuanxiong extraction is mainly concentrated in China, active substances such as essential oil, alkaloid, lactone, polysaccharide, phenols and the like are extracted from Ligusticum chuanxiong, and methods such as steam extraction, supercritical carbon dioxide extraction, solvent extraction and the like are mainly adopted, and auxiliary treatments such as heating or ultrasound are usually combined.
The Chinese patent application (application number 200710156024.6) discloses a method for obtaining ferulic acid and 3-n-butenyl phthalide by adopting solvent heating extraction, concentration and silica gel column elution combined with HPLC separation, wherein the content of the ferulic acid in the extract is about 35-45%, and the content of the 3-n-butenyl phthalide is 30-40%, but the method does not involve the determination of other components. The Chinese patent application (201710055451.9) discloses a method for preparing medicine-containing serum from an alcohol extract of ligusticum wallichii, wherein the preparation method only relates to the steps of crushing the ligusticum wallichii into powder, adding ethanol for reflux extraction, freeze-drying and crushing the obtained solid powder, and the technological parameters of the preparation method of the alcohol extract of ligusticum wallichii are not restricted in the claims. The Chinese patent application (application number 20211238098.0) discloses a method for extracting ligustilide J pure product by adopting a water solvent to extract ligusticum wallichii oil, adding potassium hydrogen peroxymonosulfate into the obtained extract to react, combining the steps of filtering, concentrating, extracting, chromatographic separation and the like, but the method does not involve the extraction and separation of other components. The Chinese patent application (application No. 20211238098.0) discloses a preparation method of a ligustilide extract, which mainly comprises the steps of crushing, soaking, extracting and purifying to obtain the ligustilide extract, wherein the ligustilide extract mainly comprises ligustilide and senkyunolide A/H/I, but the method mainly aims at separating and extracting lactone components in ligusticum wallichii. Chinese patent application (application No. 202011459453.2) discloses a preparation method of Ligusticum wallichii polysaccharide, but does not relate to preparation of other components of Ligusticum wallichii. The Chinese patent application (application number 201910543121.3) discloses a preparation method of a traditional Chinese medicine composition with the effects of activating blood circulation to dissipate blood stasis, and only describes the preparation of a crude extract of ligusticum wallichii.
Deng Peng et al (journal of pharmaceutical practice, 2020, 38 (2)) compared the differences between supercritical CO2 extraction and steam distillation of the main components of Ligusticum wallichii volatile oil; chen Wenjun (Chinese medicinal materials, 2020,43 (12)) establishes HPLC detection method of main components in herba Epimedii-rhizoma Ligustici Chuanxiong; junbo (journal of Chinese pharmacy, 2019, 54 (18)) considers that the extraction temperature and the grinding degree of medicinal materials are key influencing factors of the process for extracting the ligusticum chuanxiong volatile oil by water vapor through research. Chen Zhaoyu (International journal of Chinese medicine, 2021, 43 (12)) optimizes preparation process of vacuum vapor herbal decoction pieces of rhizoma Ligustici Chuanxiong by using ferulic acid as index, and examines antiinflammatory and analgesic activity of rhizoma Ligustici Chuanxiong herbal decoction pieces without extracting effective components of rhizoma Ligustici Chuanxiong. Ma Xiuqin et al (J.Zhongveterinarian medicine, 2020,39 (4)) established a method for quantitative nuclear magnetic resonance spectroscopy of ligustilide in Ligusticum wallichii, which did not involve extraction and optimization of the major active ingredients thereof, but the above methods did not involve application of the irradiation treatment technique in extraction of the effective ingredients of Ligusticum wallichii.
Disclosure of Invention
The application aims to solve the problems in the prior art and provides a method for improving the extraction efficiency of active ingredients of ligusticum wallichii by irradiation.
The application aims at realizing the following technical scheme:
a method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation comprises the following steps:
step one, drying ligusticum wallichii, placing the dried ligusticum wallichii in a packaging bag, sealing the packaging bag, and storing the ligusticum wallichii in a dark place;
step two, carrying out irradiation treatment on the packaged ligusticum wallichii in a normal temperature low dose mode;
step three, crushing the ligusticum wallichii after irradiation;
and step four, adding the crushed ligusticum wallichii into an extracting agent, soaking in a dark place, performing ultrasonic treatment, and filtering to obtain a supernatant.
Preferably, in the first step, the rhizoma Ligustici Chuanxiong is in form of tablet, block or powder, and is dried in a drier at 38-42deg.C for 2-4 h.
Preferably, in the first step, the packaging bag material is any one of polyethylene, nylon or aluminized film composite bag.
Preferably, in the second step, the irradiation source is selected from the group consisting of 60 Co-gamma rays or electron beams.
Preferably, in the second step, the irradiation source uses 10 MeV electron beam energy, the thickness of the bagged powder Ligusticum wallichii is not more than 5 cm when the single-sided irradiation is performed, the thickness of the flaky/blocky Ligusticum wallichii is not more than 7 cm, the thickness of the bagged powder Ligusticum wallichii is not more than 9 cm when the double-sided irradiation is performed, and the thickness of the flaky/blocky Ligusticum wallichii is 13-17 cm.
Preferably, in the second step, the absorption dose is controlled to be 1-4 kGy during the irradiation treatment.
Preferably, in the third step, the irradiated sheet-shaped/block-shaped Ligusticum wallichii is crushed by a crusher, and screened by a 40-60 mesh screen.
Preferably, in the fourth step, the crushed Ligusticum wallichii is put into a container, the extractant is added, the mixture is uniformly mixed, and the mixture is soaked for 15-30 min in dark place; placing the container into an ultrasonic device, ultrasonic treating for 20-30 min, cooling, supplementing lost weight with extractant, and filtering with 0.22 μm filter membrane to obtain supernatant.
Preferably, the extractant may be 60-80% v/v ethanol solution or 60-80% v/v methanol solution.
Preferably, the ratio of rhizoma Ligustici Chuanxiong to extractant is 1:80-200.
The beneficial effects of this technical scheme are as follows:
1. compared with the method for improving the extraction efficiency of the active ingredients of the ligusticum wallichii by irradiation, the method provided by the application has the advantages that the liquid extractant is added, and the packaging, the positioning and the like of the liquid mixed sample are fully considered during the irradiation treatment, so that the damage to the mixed sample packaging is avoided; the liquid has strong radiation shielding effect, particularly the penetration capability of electron beams in the liquid is weak, for example, irradiation and extraction are carried out simultaneously, so that the efficiency of irradiating a sample can be reduced, the irradiation treatment is not uniform easily, and the treatment effect is adversely affected; in addition, the liquid extractant can generate a large amount of free radicals after irradiation treatment, which can have adverse effect on the effective components in the system, and the defects can be effectively avoided by firstly irradiating and then extracting the raw materials. The application irradiates the raw materials, samples are in block shape, flake shape or powder shape, and the raw materials can be irradiated after being packaged, thereby being convenient and quick and having strong practicability.
2. The method for improving the extraction efficiency of the active ingredients of the ligusticum wallichii by irradiation can obviously improve the extraction yield of three active substances in the ligusticum wallichii at the same time by irradiation treatment, and widens the application range of the irradiation technology. The application limits the irradiation source, product packaging thickness, dosage range, irradiation mode, product packaging material, packaging mode and other relevant parameter ranges in irradiation processing of the ligusticum wallichii, and irradiation is required to be strictly carried out according to the parameters so as to ensure that the purpose of improving the yields of three active substances through irradiation treatment is realized.
3. The method for improving the extraction efficiency of the active ingredients of the ligusticum wallichii by irradiation provided by the application has the advantages that the active ingredients are greatly improved, and the yield improvement range is about: 10.37-21.48% of ferulic acid, 4.81-13.56% of chlorogenic acid and 6.9-24.14% of n-butylphthalide.
Detailed Description
The present application will be described in further detail with reference to examples, but embodiments of the present application are not limited thereto.
It is noted that when an element is referred to as being "mounted," "secured," or "disposed" on another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected to" another element, it can be directly connected to the other element or intervening elements may also be present.
It should be noted that, in the embodiments of the present application, terms such as left, right, up, and down are merely relative concepts or references to normal use states of the product, and should not be construed as limiting.
The content determination method of the effective components of the ligusticum wallichii comprises the following steps:
preparing standard solution stock solution, HPLC grade standard: ferulic acid (CAS 1135-24-6), chlorogenic acid (CAS 327-97-9) and n-butylphthalide (CAS 6066-49-5), precisely weighing a proper amount of standard substances, dissolving in 70% (v/v) methanol, filtering with a 0.22 μm filter membrane, and storing in dark at 4deg.C for later use, wherein the concentration range (mg/mL) of the standard substance stock solution is: 0.6-0.8 of ferulic acid, 0.5-0.7 of chlorogenic acid, and 0.5-0.8 of n-butylphthalide;
HPLC conditions for measuring the contents of ferulic acid, chlorogenic acid and n-butylphthalide in Ligusticum wallichii: u3000 chromatography, C18 column (4.6 mm ×250 mm, 5 μm), mobile phase A0.1% aqueous phosphoric acid, B acetonitrile, linear elution ladder: 0-5 min, 5-10% of B; 5-15 min, 10-30% of B; 15-20 min, 30-40% of B; 20-40 min, 40-40% B; 40-50 min, 40-80% of B; 50-60 min, 80-5% of B; 60-70 min, 5-5% of B; detection wavelengths 230 and 280 nm; the flow rate is 1.0 mL/min, the column temperature is 30 ℃, and the sample injection amount is 10 mu L;
drawing a standard curve: taking standard solution stock solutions of three standard substances, carrying out gradient dilution to obtain 6 standard solutions with different concentrations, carrying out HPLC analysis, taking the sample injection quantity (mug) as an abscissa, taking the peak area (mAU) as an ordinate, and drawing a standard curve and a linear range (mug): 0.03-0.65 ferulic acid, 0.04-0.92 chlorogenic acid, 0.01-0.21 n-butylphthalide;
the content of several active ingredients in the ligusticum wallichii before and after the irradiation treatment can be calculated through a standard curve, and the effect of the irradiation treatment on the yield of the active ingredients can be obtained.
Example 1
A method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation comprises the following steps:
step one, drying the blocky ligusticum wallichii, wherein a blast drying oven is adopted during drying, the temperature is controlled at 38 ℃, drying is carried out for 2 h, the dried ligusticum wallichii is placed in a packaging bag for sealing, the packaging bag is made of nylon, and the packaged ligusticum wallichii is stored in a dark place;
step two, carrying out irradiation treatment on the packaged ligusticum wallichii in a normal temperature low dose mode, wherein an irradiation source adopts 10 MeV electron beams, single-sided irradiation is carried out, the thickness of the ligusticum wallichii is 5 cm, and the absorption dose is controlled to be 1 kGy;
crushing the irradiated ligusticum wallichii by using a crusher, and screening by using a 40-mesh screen;
step four, putting the crushed ligusticum wallichii into a container with 0.2-g, adding an extracting agent 16-mL, adopting an ethanol solution (the ethanol concentration is 60%, v/v), uniformly mixing, and soaking for 15 min in a dark place; the vessel was placed in an ultrasonic apparatus using an ultrasonic cleaner, sonicated for 20 min, cooled, and the lost weight was made up with extractant, followed by filtration through a 0.22 μm filter to give supernatant.
Example 2
A method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation comprises the following steps:
step one, drying flaky ligusticum wallichii, wherein a forced air drying oven is adopted during drying, the temperature is controlled to be 40 ℃, the dried ligusticum wallichii is dried to be 3 h, the dried ligusticum wallichii is placed in a packaging bag for sealing, the packaging bag is made of polyethylene, and the packaged ligusticum wallichii is stored in a dark place;
step two, carrying out irradiation treatment on the packaged ligusticum wallichii in a normal-temperature low-dosage mode, wherein an irradiation source is adopted 60 Controlling the absorption dose to be 2.5 kGy during the irradiation treatment of Co-gamma rays;
crushing the irradiated ligusticum wallichii by using a crusher, and screening by using a 50-mesh screen;
step four, putting the crushed ligusticum wallichii into a container with the weight of 0.4 g, adding an extracting agent 56 mL, adopting a methanol solution (the methanol concentration is 70%, v/v), uniformly mixing, and soaking in a dark place for 25 min; the vessel was placed in an ultrasonic apparatus using an ultrasonic cleaner, sonicated for 25 min, cooled, and the lost weight was made up with extractant, followed by filtration through a 0.22 μm filter to give supernatant.
Example 3
A method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation comprises the following steps:
step one, drying flaky ligusticum wallichii, wherein a blast drying oven is adopted during drying, the temperature is controlled at 42 ℃, the dried ligusticum wallichii is dried to 4 h, the dried ligusticum wallichii is placed in a packaging bag for sealing, the packaging bag material adopts an aluminized film composite bag, and the packaged ligusticum wallichii is stored in a dark place;
step two, carrying out irradiation treatment on the packaged ligusticum wallichii in a normal-temperature low-dosage mode, wherein an irradiation source is adopted 60 Co-gamma ray, controlling suction during irradiation treatmentThe dose is 4 kGy;
step three, drying the irradiated ligusticum wallichii, crushing the ligusticum wallichii by a crusher, and screening the ligusticum wallichii by a 60-mesh screen;
step four, putting the crushed ligusticum wallichii into a container with the weight of 0.6 g, adding an extracting agent 120 mL, adopting a methanol solution (the concentration of methanol is 80%, v/v), uniformly mixing, and soaking in a dark place for 30 min; the vessel was placed in an ultrasonic apparatus using an ultrasonic cleaner, sonicated for 30 min, cooled, and the lost weight was made up with extractant, followed by filtration through a 0.22 μm filter to give supernatant.
Example 4
A method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation comprises the following steps:
step one, drying powdery ligusticum wallichii, wherein a blast drying oven is adopted during drying, the temperature is controlled at 38 ℃, drying is carried out for 2 h, the dried ligusticum wallichii is placed in a packaging bag for sealing, the packaging bag is made of nylon, and the packaged ligusticum wallichii is stored in a dark place;
step two, carrying out irradiation treatment on the packaged ligusticum wallichii in a normal temperature low dose mode, wherein an irradiation source adopts 10 MeV electron beams, double-sided irradiation is carried out, the thickness of the bagged powdery ligusticum wallichii is 9.0 cm, and the absorption dose is controlled to be 1 kGy;
step three, sieving the irradiated ligusticum wallichii with a 40-mesh screen for screening;
step four, putting the powdery ligusticum wallichii into a container with 0.2 g, adding an extracting agent 16 mL, adopting an ethanol solution (the ethanol concentration is 70%, v/v) as the extracting agent, uniformly mixing, and soaking for 15 min in a dark place; the vessel was placed in an ultrasonic apparatus using an ultrasonic cleaner, sonicated for 20 min, cooled, and the lost weight was made up with extractant, followed by filtration through a 0.22 μm filter to give supernatant.
Example 5
A method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation comprises the following steps:
step one, drying powdery ligusticum wallichii, wherein a blast drying oven is adopted during drying, the temperature is controlled at 38 ℃, drying is carried out at 1 h, the dried ligusticum wallichii is placed in a packaging bag for sealing, the packaging bag is made of an aluminized film composite bag, and the packaged ligusticum wallichii is stored in a dark place after being packaged;
step two, carrying out irradiation treatment on the packaged ligusticum wallichii in a normal temperature low dose mode, wherein an irradiation source adopts a 5.0 MeV electron beam, single-sided irradiation is carried out, the thickness of the bagged powdery ligusticum wallichii is 3 cm, and the absorption dose is controlled to be 1 kGy;
step three, sieving the irradiated ligusticum wallichii with a 40-mesh screen for screening;
step four, putting the powdery ligusticum wallichii into a container with 0.2 g, adding an extracting agent 16 mL, adopting an ethanol solution (the ethanol concentration is 80%, v/v) as the extracting agent, uniformly mixing, and soaking for 15 min in a dark place; the vessel was placed in an ultrasonic apparatus using an ultrasonic cleaner, sonicated for 20 min, cooled, and the lost weight was made up with extractant, followed by filtration through a 0.22 μm filter to give supernatant.
Example 6
A method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation comprises the following steps:
step one, drying flaky ligusticum wallichii, wherein a forced air drying oven is adopted during drying, the temperature is controlled to be 40 ℃, the drying is carried out, the ligusticum wallichii is dried to be 3 h, the dried ligusticum wallichii is placed in a packaging bag for sealing, the packaging bag is made of polyethylene, and the packaged ligusticum wallichii is stored in a dark place;
step two, carrying out irradiation treatment on the packaged ligusticum wallichii in a normal-temperature low-dosage mode, wherein an irradiation source is adopted 60 Controlling the absorption dose to be 2.5 kGy during the irradiation treatment of Co-gamma rays;
crushing the irradiated ligusticum wallichii by using a crusher, and screening by using a 50-mesh screen;
step four, putting the crushed ligusticum wallichii into a container with the weight of 0.4 and g, adding an extracting agent 56 mL, adopting a methanol solution (the methanol concentration is 60 percent, v/v), uniformly mixing, and soaking in a dark place for 25 min; the vessel was placed in an ultrasonic apparatus using an ultrasonic cleaner, sonicated for 25 min, cooled, and the lost weight was made up with extractant, followed by filtration through a 0.22 μm filter to give supernatant.
Comparative example 1
A method for extracting active ingredients of ligusticum wallichii comprises the following steps:
step one, drying the blocky ligusticum wallichii, wherein a blast drying oven is adopted during drying, the temperature is controlled at 38 ℃, drying is carried out for 2 h, the dried ligusticum wallichii is placed in a packaging bag for sealing, the packaging bag is made of nylon, and the packaged ligusticum wallichii is stored in a dark place;
step two, carrying out irradiation treatment on the packaged ligusticum wallichii in a normal temperature low dose mode, wherein an irradiation source adopts 8.0 MeV electron beam, single-sided irradiation is carried out, the thickness of the ligusticum wallichii is 4 cm, and the absorption dose is controlled to be 0.5 kGy;
crushing the irradiated ligusticum wallichii by using a crusher, and screening by using a 40-mesh screen;
step four, putting the crushed ligusticum wallichii into a container with 0.2-g, adding an extracting agent 16-mL, adopting an ethanol solution (the ethanol concentration is 60%, v/v), uniformly mixing, and soaking for 15 min in a dark place; the vessel was placed in an ultrasonic apparatus using an ultrasonic cleaner, sonicated for 20 min, cooled, and the lost weight was made up with extractant, followed by filtration through a 0.22 μm filter to give supernatant.
Comparative example 2
A method for extracting active ingredients of ligusticum wallichii comprises the following steps:
step one, drying flaky ligusticum wallichii, wherein a forced air drying oven is adopted during drying, the temperature is controlled at 35 ℃, the dried ligusticum wallichii is dried to 3 h, the dried ligusticum wallichii is placed in a packaging bag for sealing, the packaging bag is made of polyethylene, and the packaged ligusticum wallichii is stored in a dark place;
step two, carrying out irradiation treatment on the packaged ligusticum wallichii in a normal-temperature low-dosage mode, wherein an irradiation source is adopted 60 Controlling the absorption dose to be 2.5 kGy during the irradiation treatment of Co-gamma rays;
step three, drying the irradiated ligusticum wallichii, crushing the ligusticum wallichii by a crusher, and screening the ligusticum wallichii by a 50-mesh screen;
step four, putting the crushed ligusticum wallichii into a container with the weight of 0.4 g, adding an extracting agent 56 mL, adopting a methanol solution (the methanol concentration is 70%, v/v), uniformly mixing, and soaking in a dark place for 25 min; the vessel was placed in an ultrasonic apparatus using an ultrasonic cleaner, sonicated for 25 min, cooled, and the lost weight was made up with extractant, followed by filtration through a 0.22 μm filter to give supernatant.
Comparative example 3
A method for extracting active ingredients of ligusticum wallichii comprises the following steps:
step one, drying flaky ligusticum wallichii, wherein a forced air drying oven is adopted during drying, the temperature is controlled at 45 ℃, the dried ligusticum wallichii is dried to 3 h, the dried ligusticum wallichii is placed in a packaging bag for sealing, the packaging bag is made of polyethylene, and the packaged ligusticum wallichii is stored in a dark place;
step two, carrying out irradiation treatment on the packaged ligusticum wallichii in a normal-temperature low-dosage mode, wherein an irradiation source is adopted 60 Controlling the absorption dose to be 2.5 kGy during the irradiation treatment of Co-gamma rays;
step three, drying the irradiated ligusticum wallichii, crushing the ligusticum wallichii by a crusher, and screening the ligusticum wallichii by a 50-mesh screen;
step four, putting the crushed ligusticum wallichii into a container with the weight of 0.4 g, adding an extracting agent 56 mL, adopting a methanol solution (the methanol concentration is 70%, v/v), uniformly mixing, and soaking in a dark place for 25 min; the vessel was placed in an ultrasonic apparatus using an ultrasonic cleaner, sonicated for 25 min, cooled, and the lost weight was made up with extractant, followed by filtration through a 0.22 μm filter to give supernatant.
Comparative example 4
A method for extracting active ingredients of ligusticum wallichii comprises the following steps:
step one, drying powdery ligusticum wallichii, wherein a blast drying oven is adopted during drying, the temperature is controlled at 42 ℃, the drying is carried out for 4 h, the dried ligusticum wallichii is placed in a packaging bag for sealing, the packaging bag is made of an aluminized film composite bag, and the packaged ligusticum wallichii is stored in a dark place after being packaged;
step two, carrying out irradiation treatment on the packaged ligusticum wallichii in a normal-temperature low-dosage mode, wherein an irradiation source is adopted 60 Controlling the absorption dose to be 4 kGy during the irradiation treatment of Co-gamma rays;
thirdly, screening the irradiated ligusticum wallichii by a 60-mesh screen;
step four, putting the powdery ligusticum wallichii into a container with 0.6 g, adding an extracting agent 42 mL, adopting a methanol solution (the concentration of methanol is 80%, v/v), uniformly mixing, and soaking for 30 min in a dark place; the vessel was placed in an ultrasonic apparatus using an ultrasonic cleaner, sonicated for 30 min, cooled, and the lost weight was made up with extractant, followed by filtration through a 0.22 μm filter to give supernatant.
Comparative example 5
A method for extracting active ingredients of ligusticum wallichii comprises the following steps:
step one, drying flaky ligusticum wallichii, wherein a blast drying oven is adopted during drying, the temperature is controlled at 42 ℃, the dried ligusticum wallichii is dried to be 4 h, the dried ligusticum wallichii is placed in a packaging bag for sealing, the packaging bag is made of an aluminized film composite bag, and the packaged ligusticum wallichii is stored in a dark place;
step two, carrying out irradiation treatment on the packaged ligusticum wallichii in a normal-temperature low-dosage mode, wherein an irradiation source is adopted 60 Controlling the absorption dose to be 4 kGy during the irradiation treatment of Co-gamma rays;
crushing the irradiated ligusticum wallichii by using a crusher, and screening by using a 60-mesh screen;
step four, putting the crushed ligusticum wallichii into a container with the weight of 0.6 g, adding an extracting agent 160 mL, adopting a methanol solution (the concentration of methanol is 80%, v/v), uniformly mixing, and soaking in a dark place for 30 min; the vessel was placed in an ultrasonic apparatus using an ultrasonic cleaner, sonicated for 30 min, cooled, and the lost weight was made up with extractant, followed by filtration through a 0.22 μm filter to give supernatant.
Comparative example 6
A method for extracting active ingredients of ligusticum wallichii comprises the following steps:
step one, placing powdery ligusticum wallichii into a drying oven, drying, adopting a blast drying oven during drying, controlling the temperature at 38 ℃, drying 2 h, and screening by a 40-mesh screen;
step two, taking powdery ligusticum wallichii to be 0.2 and g, putting the powdery ligusticum wallichii into a container, adding an extracting agent 16 mL, adopting an ethanol solution (the ethanol concentration is 60 percent, v/v) as the extracting agent, uniformly mixing, and soaking in a dark place for 15 min; the vessel was placed in an ultrasonic apparatus using an ultrasonic cleaner, sonicated for 20 min, cooled, and the lost weight was made up with extractant, followed by filtration through a 0.22 μm filter to give supernatant.
Comparative example 7
A method for extracting active ingredients of ligusticum wallichii comprises the following steps:
step one, drying the lumpy ligusticum wallichii, adopting a blast drying oven during drying, controlling the temperature at 38 ℃, drying 2 h, crushing by a crusher, and screening by a 40-mesh screen;
step two, putting the crushed ligusticum wallichii into a container with 0.2-g, adding an extracting agent 16-mL, and soaking the extracting agent in ethanol solution (the ethanol concentration is 60%, v/v) for 15 min in a dark place; placing the container into ultrasonic equipment, ultrasonic cleaning with ultrasonic cleaner for 20 min, mixing, cooling, supplementing lost weight with extractant, sealing, performing irradiation treatment at normal temperature and low dosage, and irradiating with irradiation source 60 Co-gamma rays, controlling the absorption dose to be 1 kGy;
and step three, filtering the irradiated solution by using a 0.22 mu m filter membrane to obtain supernatant.
Comparative example 8
A method for extracting active ingredients of ligusticum wallichii comprises the following steps:
step one, drying the blocky ligusticum wallichii, wherein a blast drying oven is adopted during drying, the temperature is controlled at 38 ℃, drying is carried out for 2 h, the dried ligusticum wallichii is placed in a packaging bag for sealing, the packaging bag is made of nylon, and the packaged ligusticum wallichii is stored in a dark place;
step two, carrying out irradiation treatment on the packaged ligusticum wallichii in a normal temperature low dose mode, wherein an irradiation source adopts 10 MeV electron beams, single-sided irradiation is carried out, the thickness of the bagged ligusticum wallichii is 7 cm, and the absorption dose is controlled to be 1 kGy;
crushing the irradiated ligusticum wallichii by using a crusher, and screening by using a 40-mesh screen;
step four, putting the crushed ligusticum wallichii into a container with 0.2-g, adding an extracting agent 16-mL, adopting an ethanol solution (the ethanol concentration is 50%, v/v), uniformly mixing, and soaking for 15 min in a dark place; the vessel was placed in an ultrasonic apparatus using an ultrasonic cleaner, sonicated for 20 min, cooled, and the lost weight was made up with extractant, followed by filtration through a 0.22 μm filter to give supernatant.
Comparative example 9
A method for extracting active ingredients of ligusticum wallichii comprises the following steps:
step one, drying the blocky ligusticum wallichii, wherein a blast drying oven is adopted during drying, the temperature is controlled at 38 ℃, drying is carried out for 2 h, the dried ligusticum wallichii is placed in a packaging bag for sealing, the packaging bag is made of nylon, and the packaged ligusticum wallichii is stored in a dark place;
step two, carrying out irradiation treatment on the packaged ligusticum wallichii in a normal temperature low dose mode, wherein an irradiation source adopts 10 MeV electron beams, single-sided irradiation is carried out, the thickness of the bagged ligusticum wallichii is 5 cm, and the absorption dose is controlled to be 1 kGy;
crushing the irradiated ligusticum wallichii by using a crusher, and screening by using a 40-mesh screen;
step four, putting the crushed ligusticum wallichii into a container with 0.2-g, adding an extracting agent 16-mL, adopting an ethanol solution (the ethanol concentration is 85%, v/v), uniformly mixing, and soaking for 15 min in a dark place; the vessel was placed in an ultrasonic apparatus using an ultrasonic cleaner, sonicated for 20 min, cooled, and the lost weight was made up with extractant, followed by filtration through a 0.22 μm filter to give supernatant.
The content of the effective components of Ligusticum wallichii was measured in examples 1-6 and comparative examples 1-9, and the specific data are shown in the following table:
from the examination of examples 1 to 6 and comparative examples 1 to 9, it is known that irradiation sources, product packaging thickness, dose ranges, irradiation modes, product packaging materials, packaging modes and other related parameter ranges in irradiation processing of a specific Ligusticum chuanxiong are required to be subjected to irradiation treatment, and irradiation is strictly required to be performed according to the parameters, so that the purpose of improving the yields of three active substances through irradiation treatment can be achieved.
The foregoing description is only a preferred embodiment of the present application, and is not intended to limit the present application in any way, and any simple modification, equivalent variation, etc. of the above embodiment according to the technical matter of the present application fall within the scope of the present application.
Claims (5)
1. A method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation is characterized by comprising the following steps:
step one, drying ligusticum wallichii, placing the dried ligusticum wallichii in a packaging bag, sealing the packaging bag, and storing the ligusticum wallichii in a dark place; drying rhizoma Ligustici Chuanxiong in drier at 38-42deg.C for 2-4 h;
step two, carrying out irradiation treatment on the packaged ligusticum wallichii in a normal temperature low dose mode; the irradiation source adopts 60 Co-gamma rays; during the irradiation treatment, controlling the absorption dose to be 1-4 kGy;
step three, crushing the ligusticum wallichii after irradiation;
step four, adding the crushed ligusticum wallichii into an extracting agent, soaking in a dark place, performing ultrasonic treatment, and filtering to obtain a supernatant; placing crushed rhizoma Ligustici Chuanxiong into a container, adding extractant, mixing, and soaking in dark place for 15-30 min; placing the container into an ultrasonic device, performing ultrasonic treatment for 20-30 min, cooling, supplementing lost weight with extractant, and filtering with 0.22 μm filter membrane to obtain supernatant; the ratio of rhizoma Ligustici Chuanxiong to extractant is 1:80-200.
2. A method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation is characterized by comprising the following steps:
step one, drying ligusticum wallichii, placing the dried ligusticum wallichii in a packaging bag, sealing the packaging bag, and storing the ligusticum wallichii in a dark place; drying rhizoma Ligustici Chuanxiong in drier at 38-42deg.C for 2-4 h;
step two, carrying out irradiation treatment on the packaged ligusticum wallichii in a normal temperature low dose mode; the irradiation source adopts electron beams; under the condition of adopting 10 MeV electron beam energy, the thickness of the bagged powdery Ligusticum wallichii is not more than 5 cm when in single-sided irradiation, the thickness of the flaky/blocky Ligusticum wallichii is not more than 7 cm, the thickness of the bagged powdery Ligusticum wallichii is not more than 9 cm when in double-sided irradiation, and the thickness of the flaky/blocky Ligusticum wallichii is 13-17 cm; during the irradiation treatment, controlling the absorption dose to be 1-4 kGy;
step three, crushing the ligusticum wallichii after irradiation;
step four, adding the crushed ligusticum wallichii into an extracting agent, soaking in a dark place, performing ultrasonic treatment, and filtering to obtain a supernatant; placing crushed rhizoma Ligustici Chuanxiong into a container, adding extractant, mixing, and soaking in dark place for 15-30 min; placing the container into an ultrasonic device, performing ultrasonic treatment for 20-30 min, cooling, supplementing lost weight with extractant, and filtering with 0.22 μm filter membrane to obtain supernatant; the ratio of rhizoma Ligustici Chuanxiong to extractant is 1:80-200.
3. The method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation according to claim 1 or 2, wherein the method comprises the following steps: in the first step, the packaging bag material is any one of polyethylene, nylon or aluminized film composite bags.
4. The method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation according to claim 1 or 2, wherein the method comprises the following steps: in the third step, the irradiated block or sheet Ligusticum wallichii is crushed by a crusher, and screened by a 40-60 mesh screen.
5. The method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation according to claim 1 or 2, wherein the method comprises the following steps: the extractant can be 60-80% v/v ethanol solution or 60-80% v/v methanol solution.
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| CN103755507A (en) * | 2014-02-21 | 2014-04-30 | 湖北省农业科学院农产品加工与核农技术研究所 | Method for extracting plant total flavones through normal-temperature low-dosage irradiation |
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| CN103755507A (en) * | 2014-02-21 | 2014-04-30 | 湖北省农业科学院农产品加工与核农技术研究所 | Method for extracting plant total flavones through normal-temperature low-dosage irradiation |
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