CN113350459A - A method for preparing Chinese medicinal oral liquid for treating lung cancer and quality control method thereof - Google Patents
A method for preparing Chinese medicinal oral liquid for treating lung cancer and quality control method thereof Download PDFInfo
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- CN113350459A CN113350459A CN202110477120.0A CN202110477120A CN113350459A CN 113350459 A CN113350459 A CN 113350459A CN 202110477120 A CN202110477120 A CN 202110477120A CN 113350459 A CN113350459 A CN 113350459A
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Abstract
The invention discloses a preparation method and a quality control method of traditional Chinese medicine oral liquid for treating lung cancer. The invention selects two Chinese medicines of ginseng and coix seed, and the finished product is prepared by the steps of decoction, filtration, concentration, alcohol precipitation, preparation, three-phase separation, filtration and the like. The invention adopts the membrane separation technology, adds the ultrafiltration process, obtains clear and transparent liquid, removes macromolecular impurities such as microorganisms, proteins and the like in the solution, and greatly improves the quality and the stability of the product. Solves the problems of turbidity and easy precipitation of the liquid medicine in the prior art, optimizes the process of the product, improves the taste of the product, uses less raw materials, has simple process operation and is suitable for industrial production. The traditional Chinese medicine oral liquid disclosed by the invention has the effects of tonifying spleen and benefiting lung, is used for combined administration during chemotherapy of patients with lung cancer of qi deficiency, can obviously improve symptoms such as physical weakness and hypodynamia, short breath and spontaneous perspiration, inappetence and the like, has no toxic or side effect, and is beneficial to popularization and application.
Description
Technical Field
The invention relates to a preparation method and a quality control method of traditional Chinese medicine oral liquid for treating lung cancer, belonging to the technical field of medicines.
Background
Ginseng radix is dried root and rhizome of Panax ginseng C.A.Mey. of Araliaceae, and has effects of invigorating primordial qi, recovering pulse, relieving depletion, invigorating spleen, benefiting lung, promoting fluid production, nourishing blood, tranquilizing mind, and improving intelligence. Can be used for treating asthenia, collapse, cold limbs, weak pulse, spleen deficiency, anorexia, lung deficiency, cough, asthma, thirst due to body fluid consumption, internal heat, asthenia, palpitation, insomnia, sexual impotence, and cold womb. The Shen nong Ben Cao Jing records that ginseng tonifies five internal organs, calms spirit, stops palpitation, removes pathogenic factors, improves eyesight, and benefits intelligence. Modern pharmacological research finds that ginseng contains various chemical components, contains ginsenoside, ginseng polysaccharide, polypeptide, fatty acid, amino acid, polyacetylene alcohol and the like, and has the effects of enhancing immunity, resisting fatigue and virus, assisting in treating malignant tumors and the like.
Ginseng is used as a raw material, effective components are extracted by a percolation method to prepare the ginseng oral liquid, and the ginseng oral liquid has the special fragrance of the ginseng and slightly bitter taste. Has effects of invigorating primordial qi, promoting fluid production, and quenching thirst. Can be used for treating asthenia, anorexia, palpitation, short breath, insomnia, and amnesia.
Ginseng radix has antifatigue and immunity enhancing effects. Wangzhen and the like research the effect of the compound ginseng extract on relieving physical fatigue. The effect of the compound ginseng extract on alleviating physical fatigue is observed through the influence on the weight-bearing swimming time of mice and the content of serum urea, hepatic glycogen and blood lactic acid. Results the mice in the experimental group had significantly longer swimming times than the control group, and were statistically significant (P < 0.05). The ginseng extract can obviously enhance the adaptability of the body to the exercise load and resist the generation of fatigue. The Zhouyihong research shows that the group with the dosages of 120mg/kg and 240mg/kg of total ginsenoside (SPG) can improve the spleen index and the thymus index of mice with low immunity, wherein the high-dosage SPG can well protect the cellular immunity and the humoral immunity of the organism. For example, two dosage groups of SPG can obviously improve the phagocytic capacity of reticuloendothelial system and the phagocytic capacity of mononuclear-macrophage of mice under immune hypofunction induced by cyclophosphamide and promote the nonspecific immune function of the mice under immune hypofunction.
The ginsenoside has adjuvant therapeutic effect on malignant tumor. The clinical observation of ginsenoside induced apoptosis in rectal cancer cells was conducted by the method of Shichen Jianhua and the like. Results the clinical symptoms of the treatment group were improved after the administration, and 23 cases (65.7%) showed that the ultrastructure of most cancer cells was similar to that of the control group, but apoptotic cancer cells were clearly observed among the cancer cells. The clinical symptoms of the control group are not obviously improved, necrotic cancer cells can be seen under an electron microscope, and apoptotic cancer cells are not observed. The ginsenoside is suggested to have a better auxiliary effect on inducing the rectal cancer cell apoptosis. Chengmiwei and the like observe the clinical auxiliary curative effect of the ginsenoside 20(R) -Rg3 on lung cancer. The treatment group chemotherapy is administered with ginsenoside 20(R) -Rg3, 20mg 2 times daily; the control group was observed for 6-8 weeks with chemotherapy alone. The effective rate of the result treatment group is obviously higher than that of the control group, the life quality is obviously improved, the weight is increased, and the functions of the heart, the liver and the kidney are not obviously changed. The ginsenoside 20(R) -Rg3 is shown to have better auxiliary curative effect on lung cancer.
Coix seed, commonly known as Coix seed, is a dry mature seed of Coix seed. Coix seed is an annual or perennial herbaceous plant, Gramineae, an ancient medical and edible precious variety in China, and is one of 87 substances listed in food and medicines published by the Ministry of health as early as 2002. Li Shizhen is in the cloud of Ben Cao gang mu: "Xiaoke Drinking Water" and Yi ren boiled porridge. "further: the coix seed porridge has the functions of removing damp-heat and benefiting intestines and stomach. The Qing, Chen Shi ze toll (New compilation of materia Medica) records that Coix lacryma-joli is sweet in taste, slightly cold in smell and non-toxic. The coix seed porridge is beneficial to the patients with weak health caused by long-term illness, the recovery period after delivery, the old, children and the like. Coicis semen has effects of promoting diuresis, eliminating dampness, invigorating spleen, relieving diarrhea, eliminating arthralgia, expelling pus, removing toxic substance, and resolving hard mass, and can be used for treating edema, loempe, dysuresia, spleen deficiency, diarrhea, damp arthralgia, spasm, pulmonary abscess, intestinal abscess, wart, cancer, etc. Coicis semen contains functional components such as polysaccharide compound, ester compound and triterpene compound, and has pharmacological effects of resisting tumor, resisting inflammation, improving immunity, and lowering blood sugar.
The coix seeds have the function of improving the immunity, and the studies on the immune regulation function of the coix seed water extract on the low-immune mice caused by cyclophosphamide are carried out by leaf sensitivity researches, so that the coix seed water extract can improve the immune organ weight index of the low-immune mice caused by cyclophosphamide, improve the leukocyte number and the phagocytosis percentage and phagocytosis index of immunosuppressive mice, increase the content of serum hemolysin and increase the positive rate of T lymphocyte esterase of the immunosuppressive mice, and prompt that the coix seed water extract can improve the humoral immunity and cellular immunity of organisms; the effect of the coix seed polysaccharide on the immune function of a mouse is observed by Miao Ming three observations, and the coix seed polysaccharide with different concentrations is administrated after gastric lavage on a cyclophosphamide established low-immune model mouse, so that the result shows that the coix seed polysaccharide can improve the phagocytosis percentage and the phagocytosis index of macrophages in the abdominal cavity of the mouse, promote the formation of hemolysin and hemolytic plaques and promote the lymphocyte transformation; the influence of the coix seed oil on the immune function of the mouse is discussed by perikarya fei and the like, and the observation shows that the high dose of the coix seed oil can obviously enhance the proliferation capability of spleen lymphocytes and delayed allergic reaction, increase the serum hemolysin level of the mouse, enhance the antibody generating capability and NK cell activity of the mouse and have the function of enhancing the immunity.
Coicis semen has effect in relieving physical fatigue. Xiaozhiyong is to observe the antibody fatigue effect of coix seed polysaccharide, and after different doses of coix seed polysaccharide are given to a mouse, a heavy swimming test and the measurement of serum urea, blood lactic acid and liver glycogen are carried out on the mouse, so that the coix seed polysaccharide can prolong the heavy swimming time of the mouse, reduce the generation of the serum urea of the mouse during exercise, increase the liver glycogen content of the mouse, prompt that the coix seed polysaccharide has the capability of improving the adaptability of an organism to exercise load, and has obvious effects on delaying the generation of physical fatigue and accelerating the elimination of fatigue.
The Kanleit injection is an anticancer active compound extracted and separated from the traditional Chinese medicine semen coicis by applying modern scientific technology, and has the effects of promoting diuresis, permeating moisture, strengthening spleen, tonifying lung, clearing heat, removing arthralgia, detoxifying and dissipating binds. The patient is given with the Conlet injection for 30 days as a treatment course, and the change of blood routine, kps score, T cell subgroup change and the like of the patient is observed after treatment. Results 32 patients PR 9, PD 13, NC 10. The KPS score improved from the average 52 points before treatment to 74 points, 9 of 12 pain patients were relieved, 2 were relieved completely, and the total effective rate was 75%. The liver and kidney function has no obvious change before and after treatment. T cell subsets changed significantly after treatment. Is one of the more ideal anti-tumor drugs in the current tumor comprehensive treatment, and is worthy of further research, popularization and application.
Lung cancer belongs to the categories of cough, pulmonary abscess, hemoptysis, chest pain and the like in traditional Chinese medicine, and ancient documents refer to lung accumulation, stomach ache and the like. In the book of difficult classic, "cough with dyspnea, even with superficial and adverse rise of qi due to saliva … …". Also, the accumulation of lung, named as Xie cardia, is just as big as a cup under the right hypochondrium and causes cough, dyspnea and cough with lung congestion. Phlegm is similar to fluid but different in name, thick and turbid is clear and thin, and is the result of accumulation of dampness. But the dampness also originates from the spleen, so it is said that the spleen is the source of phlegm generation and the lung is the device for storing phlegm. Therefore, it should not be treated with phlegm alone, so the root of phlegm should be treated. Ginseng has the effects of tonifying spleen and lung, promoting the production of body fluid and nourishing blood, and Coicis semen has the effects of promoting diuresis, eliminating dampness, invigorating spleen and relieving diarrhea. The combination of the two has certain curative effect on the elderly, weak and lung cancer patients with lung and spleen deficiency.
The Chinese medicinal composition for treating the lung cancer consists of two medicaments of ginseng and coix seed, and has the following functions and main indications: to invigorate the spleen and nourish the lung. Is used for the combined application of chemotherapy for patients with lung cancer with qi deficiency. Can be used for treating asthenia, short breath, spontaneous perspiration, and anorexia. The patent application with the publication number of CN 1615917A discloses a combined medicine for advanced cancer or chemotherapy and a preparation method thereof, and relates to a medicine which consists of two components, namely ginseng and coix seed, wherein the weight fractions of the two components are one part of ginseng and 4-6 parts of coix seed. However, after the traditional Chinese medicine composition for treating lung cancer is added with the water preparation, the traditional Chinese medicine composition has an obvious amount of oily substances, is yellow and slightly sticky, can not be intercepted by common filtration, seriously influences the appearance state of a finished product, and is turbid and not clear. The preparation method comprises pulverizing the raw materials into coarse powder, and decocting in water. By adopting the direct extraction method, the water solution can not fully infiltrate the interior, and the extraction is not sufficient.
Therefore, the invention provides a preparation method and a quality control method of a traditional Chinese medicine composition for treating lung cancer. Through the membrane separation technology, macromolecular impurities such as microorganisms and proteins in the solution are removed, and the quality and stability of the product are greatly improved. Solves the problems of turbidity and easy precipitation of the liquid medicine in the prior art, and optimizes the process of the product. Secondly, the invention adopts a mode of extraction after soaking to carry out feeding production. The amount of the concentrated extract of the extracting solution is obviously increased, and the active substance components are increased.
Disclosure of Invention
The invention aims to provide a preparation method and a quality control method of traditional Chinese medicine oral liquid for treating lung cancer.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention relates to a preparation method of a traditional Chinese medicine oral liquid for treating lung cancer, which comprises the following steps:
(1) low-temperature crushing and weighing:
pulverizing ginseng and coix seeds into coarse powder at a low temperature of 0-15 ℃, sieving the coarse powder by a 20-100-mesh sieve, and weighing the coarse powder according to the proportion of 0.5-3 parts by weight of ginseng and 1-9 parts by weight of coix seeds;
(2) decocting and filtering:
wrapping the pulverized medicinal materials with filter cloth, soaking in water, decocting with water twice, the first time with 11-13 times of water for 1-2 hr, the second time with 7-9 times of water for 0.5-1.5 hr, mixing decoctions, and filtering;
(3) concentrating and recovering ethanol:
concentrating the filtrate to relative density of 1.18-1.22 at 50 deg.C, adding 2 times volume of ethanol, standing for 10-12 hr, collecting supernatant, and recovering ethanol until no ethanol smell exists;
(4) three-phase separation:
adding water to the prescribed amount, performing three-phase separation by using a three-phase butterfly separator, and taking heavy-phase liquid for later use;
(5) and (3) filtering:
filtering the heavy phase liquid by using a micro-filter, and ultrafiltering the filtrate by using a hollow fiber ceramic membrane with the molecular weight cutoff of 30-80 kDa, wherein the filtrate is for later use;
(6) filling and sealing, and sterilizing:
and (5) taking the filtrate obtained in the step (5), filling and sealing, and sterilizing to obtain the traditional Chinese medicine.
Preferably, the crude powder is weighed according to the proportion of 1 part by weight of ginseng and 4-6 parts by weight of coix seeds, and more preferably, the crude powder is weighed according to the proportion of 1 part by weight of ginseng and 5 parts by weight of coix seeds.
Preferably, the production capacity of the three-phase butterfly separator is 50-150L/h, the temperature is 20-30 ℃, the pressure of a material inlet is 0-0.1MPa, and the pressure of a material outlet is 0-0.3 MPa.
Wherein, preferably, the micro-filtration membrane aperture of the micro-filtration machine is 0.2-1.0 μm, the working pressure is 0.10-0.6Mpa, the flow rate is 5-30t/h, and the temperature is 20-60 ℃.
Wherein, preferably, the transmembrane pressure difference of the ultrafiltration is 0.1-0.5mpa, the flow rate is 1.0-5.0m/s, and the temperature is 50-80 ℃.
Among them, the prescribed amount is preferably 5 parts by weight.
Preferably, the preparation method further comprises the step of controlling the quality of the prepared traditional Chinese medicine oral liquid, and the method comprises the following steps:
(1) preparation of control solutions:
accurately weighing appropriate amount of ginsenoside Rg1 and ginsenoside Re reference substances, adding methanol to obtain reference substance solution containing ginsenoside Rg10.5mg or ginsenoside Re0.4mg per 1ml, and shaking;
(2) preparation of a test solution:
precisely measuring 20ml of the prepared traditional Chinese medicine oral liquid, placing the oral liquid in a split-flow funnel, adding 10ml of water, extracting with chloroform for 2 times, 10ml each time, discarding chloroform solution, extracting the water solution with saturated n-butanol for 4 times, 25ml each time, performing ultrasonic treatment for 60min, filtering, evaporating n-butanol solution to dryness, dissolving the residue with methanol, transferring the dissolved residue to a 5ml measuring flask, adding methanol to scale, and shaking up to obtain the traditional Chinese medicine oral liquid;
(3) and (3) determination:
respectively sucking 10ul of each of the two reference substance solutions and the sample solution, injecting into a liquid chromatograph, and measuring under the following chromatographic conditions:
filling agent: octadecylsilane chemically bonded silica;
mobile phase: the volume ratio of 99:400 acetonitrile-0.05% phosphoric acid solution as mobile phase;
detection wavelength: 200-250 nm;
the number of theoretical plates: calculated according to the peak of ginsenoside Re, should not be lower than 2500.
Among them, it is preferable that the detection wavelength in the step (3) is 203 nm.
Preferably, the preparation method further comprises the step of identifying the prepared traditional Chinese medicine oral liquid, and the method comprises the following steps:
(1) the thin-layer identification of ginsenoside Re as the marker component of ginseng comprises the following steps:
1) preparing a test solution:
taking 10ml of the prepared traditional Chinese medicine oral liquid, adding 10ml of water, placing in a separating funnel, extracting with chloroform for 2 times, 10ml each time, discarding chloroform solution, extracting aqueous solution with water saturated n-butanol for 2 times, 30ml each time, combining n-butanol solution, adding ammonia test solution 30ml, shaking uniformly, standing for layering, collecting n-butanol solution, washing with water for 2 times, 40ml each time, discarding water solution, evaporating n-butanol solution to dryness, and adding methanol 1ml to residue for dissolving to obtain sample solution;
2) preparation of a reference substance: adding methanol into ginsenoside Re reference substance to obtain 2ml solution per 1ml as reference substance solution;
3) the identification method comprises the following steps:
according to the thin layer chromatography test, 5ul of each of the test solution and the reference solution is sucked and respectively spotted on the same silica gel G thin layer plate according to the volume ratio of 15: 40: 22: 10 chloroform-ethyl acetate-methanol-aqueous solution, taking the lower layer solution placed below 10 ℃ as a developing agent, developing, taking out, airing, spraying 10% sulfuric acid ethanol solution, heating at 105 ℃ until the color of the spots is clearly developed, respectively inspecting under sunlight and 365nm ultraviolet light, and displaying the spots or glowworm spots with the same color in the chromatogram of the test sample at the positions corresponding to the chromatogram of the reference sample;
(2) the method for identifying the marker component of the coix seed, namely the glycerol trioleate, comprises the following steps:
1) preparation of control solutions:
taking 10mg of triolein reference substance, precisely weighing, placing into a 10mL measuring flask, and adding petroleum ether to prepare 1mL solution containing 1mg of triolein to obtain the final product;
2) preparation of a test solution:
taking a coix seed raw material for preparing the traditional Chinese medicine oral liquid, crushing, weighing 1g of powder, adding 10mL of petroleum ether, carrying out ultrasonic treatment for 30min, filtering, evaporating filtrate to dryness, and dissolving residues in 1mL of petroleum ether to obtain a sample solution;
3) preparing a reference medicinal material solution:
precisely weighing semen Coicis reference material 1g, adding petroleum ether 10mL, ultrasonic treating for 30min, filtering, evaporating filtrate, and dissolving residue with petroleum ether 1mL to obtain semen Coicis reference material solution;
4) the identification method comprises the following steps:
adopting thin layer chromatography, selecting silica gel G as stationary phase, using 0.5% w/w sodium carboxymethylcellulose solution as adhesive, respectively absorbing 10uL of each of glyceryl trioleate reference solution, test sample solution and reference medicinal material solution, dropping on silica gel G plate, and dispensing with a volume ratio of 25: 5: 1, spreading to 15cm, taking out, air drying, spraying 0.5% vanillin-98% concentrated sulfuric acid ethanol solution, heating at 105 deg.C for 5min, and inspecting under 365nm ultraviolet lamp to obtain clear spots, wherein the chromatogram of Coicis semen sample, reference substance and reference material shows identical fluorescence spots.
Furthermore, the invention also provides the traditional Chinese medicine oral liquid prepared by the method. And
the traditional Chinese medicine oral liquid is applied to the preparation of the medicine for treating lung cancer and/or reducing weight.
Compared with the prior art, the invention has the beneficial effects that:
1. the traditional Chinese medicine injection can generate certain adverse reactions due to the allergy of organisms to medicines, poor stability of components, medicine stimulation and improper infusion operation. The product of the invention is used as an oral liquid preparation, is safe without toxic and side effects, has simple administration method, and is a better medicament for adjuvant therapy of lung cancer.
2. The invention only selects two traditional Chinese medicines of ginseng and coix seed, and the finished product is prepared by the steps of decoction, filtration, concentration, alcohol precipitation, preparation, three-phase separation, filtration and the like. The raw materials are few, the process operation is simple, and the method is suitable for industrial production.
3. The product of the invention has the effects of strengthening spleen and benefiting lung, is used for combined administration during chemotherapy of patients with lung cancer of qi deficiency, can obviously improve symptoms such as weakness and hypodynamia, short breath and spontaneous perspiration, inappetence and the like, has no toxic or side effect, and is beneficial to popularization and application.
4. The invention adopts the membrane separation technology, adds the ultrafiltration process, obtains clear and transparent liquid, removes macromolecular impurities such as microorganisms, proteins and the like in the solution, and greatly improves the quality and the stability of the product. Solves the problems of turbidity and easy precipitation of the liquid medicine in the prior art, and optimizes the process of the product. Improves the mouth feel of the product.
Detailed Description
In order to more clearly illustrate the technical solutions in the implementation process of the present invention, the present invention is further described in detail with reference to the following examples, which are illustrative of the present invention and do not limit the scope of the present invention.
Example 1 preparation of a Chinese medicinal oral liquid for treating lung cancer
(1) Low-temperature crushing and weighing:
pulverizing Ginseng radix and Coicis semen at 5 deg.C into coarse powder, sieving with 80 mesh sieve, and weighing coarse powder according to the weight ratio of 1 part of Ginseng radix and 5 parts of Coicis semen;
(2) decocting and filtering:
wrapping the pulverized medicinal materials with filter cloth, soaking in water, decocting with water twice, first with 12 times of water for 1.5 hr, second with 8 times of water for 1 hr, mixing decoctions, and filtering;
(3) concentrating and recovering ethanol:
concentrating the filtrate to relative density of 1.2 at 50 deg.C, adding 2 times volume of ethanol, standing for 12 hr, collecting supernatant, and recovering ethanol until no alcohol smell exists;
(4) three-phase separation:
adding water to the amount of 5 parts by weight, performing three-phase separation by using a three-phase butterfly separator (with the production capacity of 100L/h, the temperature of 20 ℃, the pressure of a material inlet of 0.1MPa and the pressure of a material outlet of 0.3MPa), and taking heavy-phase liquid for later use;
(5) and (3) filtering:
filtering the heavy phase liquid by a microfiltration machine (the aperture of a microfiltration membrane is 1.0 mu m, the working pressure is 0.10Mpa, the flow rate is 15t/h, the temperature is 50 ℃), and ultrafiltering the filtrate by a hollow fiber ceramic membrane with the molecular weight cutoff of 50kDa (the transmembrane pressure difference is 0.3Mpa, the flow rate is 1.0m/s, the temperature is 50 ℃), wherein the filtrate is reserved;
(6) filling and sealing, and sterilizing:
and (5) taking the filtrate obtained in the step (5), filling and sealing according to 10ml per bottle, and sterilizing to obtain the traditional Chinese medicine.
Example 2 preparation of a Chinese medicinal oral liquid for treating lung cancer
(1) Low-temperature crushing and weighing:
pulverizing Ginseng radix and Coicis semen at 10 deg.C into coarse powder, sieving with 50 mesh sieve, and weighing coarse powder according to the proportion of 2 weight parts of Ginseng radix and 5 weight parts of Coicis semen;
(2) decocting and filtering:
wrapping the pulverized medicinal materials with filter cloth, soaking, decocting with 11 times of water for 2 hr, decocting with 7 times of water for 1.5 hr, mixing decoctions, and filtering;
(3) concentrating and recovering ethanol:
concentrating the filtrate to relative density of 1.18-1.22 at 50 deg.C, adding 2 times volume of ethanol, standing for 12 hr, collecting supernatant, and recovering ethanol until no ethanol smell exists;
(4) three-phase separation:
adding water to the amount of 5 parts by weight, performing three-phase separation with a three-phase butterfly separator (production capacity of 100L/h, temperature of 20 deg.C, material inlet pressure of 0.1mpa, and material outlet pressure of 0.3mpa), and collecting heavy phase liquid for use.
(5) And (3) filtering:
filtering the heavy phase liquid by a microfiltration machine (the aperture of a microfiltration membrane is 1 mu m, the working pressure is 0.10Mpa, the flow rate is 15t/h, the temperature is 50 ℃), and ultrafiltering the filtrate by a hollow fiber ceramic membrane with the molecular weight cutoff of 30kDa (the transmembrane pressure difference is 0.3Mpa, the flow rate is 1.0m/s, the temperature is 50 ℃), wherein the filtrate is reserved.
(6) Filling and sealing, and sterilizing:
packaging the above filtrate at a ratio of 10 ml/bag, and sterilizing.
EXAMPLE 3 preparation of Chinese medicinal oral liquid for treating Lung cancer
(1) Low-temperature crushing and weighing:
pulverizing Ginseng radix and Coicis semen at 8 deg.C into coarse powder, sieving with 100 mesh sieve, and weighing coarse powder according to the weight ratio of 1.5 parts of Ginseng radix and 6 parts of Coicis semen;
(2) decocting and filtering:
wrapping the pulverized medicinal materials with filter cloth, soaking, decocting with water twice, first with 12 times of water for 1.5 hr, and second with 8 times of water for 1.0 hr, mixing decoctions, and filtering;
(3) concentrating and recovering ethanol:
concentrating the filtrate to relative density of 1.18-1.22 at 50 deg.C, adding 2 times of ethanol, standing for 12 hr, collecting supernatant, and recovering ethanol until no alcohol smell exists;
(4) three-phase separation:
adding water to the amount of 5 parts by weight, performing three-phase separation with a three-phase butterfly separator at a speed of 120L/h and a temperature of 20 ℃, under a pressure of 0.1mpa at a material inlet and under a pressure of 0.3mpa at a material outlet, and collecting heavy phase liquid for later use.
(5) And (3) filtering:
filtering the heavy phase liquid by a microfiltration machine (the aperture of a microfiltration membrane is 0.45 mu m, the working pressure is 0.10Mpa, the flow rate is 10t/h and the temperature is 40 ℃), and ultrafiltering the filtrate by a hollow fiber ceramic membrane with the molecular weight cutoff of 50kDa (the transmembrane pressure difference is 0.35Mpa, the flow rate is 2.0m/s and the temperature is 60 ℃), wherein the filtrate is reserved.
(6) Filling and sealing, and sterilizing:
packaging the above filtrate at a ratio of 10 ml/bag, and sterilizing.
Example 4 preparation of a Chinese medicinal oral liquid for treating lung cancer
(1) Low-temperature crushing and weighing:
pulverizing Ginseng radix and Coicis semen at 10 deg.C into coarse powder, sieving with 60 mesh sieve, and weighing coarse powder according to the weight ratio of 2 parts of Ginseng radix and 7 parts of Coicis semen;
(2) decocting and filtering:
wrapping the pulverized materials with filter cloth, soaking, decocting with water twice, first with 12 times of water for 1.5 hr, and second with 8 times of water for 1 hr, mixing decoctions, and filtering.
(3) Concentrating and recovering ethanol:
concentrating the filtrate to relative density of 1.18-1.22 at 50 deg.C, adding 2 times volume of ethanol, standing for 12 hr, collecting supernatant, and recovering ethanol until no alcohol smell is obtained.
(4) Three-phase separation:
adding water to the amount of 5 parts by weight, performing three-phase separation with a three-phase butterfly separator at a speed of 100L/h and a temperature of 20 ℃, under a pressure of 0.05mpa at a material inlet and under a pressure of 0.2mpa at a material outlet, and collecting heavy-phase liquid for later use.
(5) And (3) filtering:
filtering the heavy phase liquid by a microfiltration machine (the aperture of a microfiltration membrane is 1 mu m, the working pressure is 0.10Mpa, the flow rate is 10t/h, the temperature is 60 ℃), and ultrafiltering the filtrate by a hollow fiber ceramic membrane with the molecular weight cutoff of 80kDa (the transmembrane pressure difference is 0.4Mpa, the flow rate is 3.0m/s, the temperature is 50 ℃), wherein the filtrate is reserved.
(6) Filling and sealing, and sterilizing:
packaging the above filtrate at a ratio of 10 ml/bag, and sterilizing.
EXAMPLE 5 preparation of Chinese medicinal oral liquid for treating Lung cancer
(1) Low-temperature crushing and weighing:
pulverizing Ginseng radix and Coicis semen at 10 deg.C into coarse powder, sieving with 80 mesh sieve, and weighing coarse powder according to the weight ratio of 2.5 parts of Ginseng radix and 9 parts of Coicis semen;
(2) decocting and filtering:
wrapping the pulverized materials with filter cloth, soaking, decocting with water twice, first with 13 times of water for 1.5 hr, and second with 8 times of water for 1 hr, mixing decoctions, and filtering.
(3) Concentrating and recovering ethanol:
concentrating the filtrate to relative density of 1.18-1.22 at 50 deg.C, adding 2 times volume of ethanol, standing for 12 hr, collecting supernatant, and recovering ethanol until no alcohol smell is obtained.
(4) Three-phase separation:
adding water to the amount of 5 parts by weight, performing three-phase separation with a three-phase butterfly separator at a speed of 100L/h and a temperature of 20 ℃, under a pressure of 0.1mpa at a material inlet and under a pressure of 0.3mpa at a material outlet, and collecting heavy phase liquid for later use.
(5) And (3) filtering:
filtering the heavy phase liquid by a microfilter (the aperture of a microfiltration membrane is 1 mu m, the working pressure is 0.10Mpa, the flow rate is 10t/h, the temperature is 60 ℃) and carrying out ultrafiltration on the filtrate by a hollow fiber ceramic membrane with the molecular weight cutoff of 30kDa (the transmembrane pressure difference is 0.4Mpa, the flow rate is 3.0m/s, and the temperature is 60 ℃).
(6) Filling and sealing, and sterilizing:
packaging the above filtrate at a ratio of 10 ml/bag, and sterilizing.
EXAMPLE 6 optimization and establishment of the method
1. Selection of conditions for pulverizing raw materials
A Chinese medicinal oral liquid for treating lung cancer is prepared from Ginseng radix and Coicis semen by pulverizing. According to the comparison of the ginsenoside contents (ginsenoside Rg1 and ginsenoside Re) in the coarse powder in different grinding modes, proper grinding conditions are selected, and the experimental results are shown as follows.
TABLE 1 Effect of different comminution methods on the product
And (4) conclusion: from experimental results, compared with normal-temperature crushing, the contents of effective components ginsenoside Rg1 and ginsenoside Re are higher under the low-temperature crushing condition. Thus, the low-temperature pulverization is superior to the normal-temperature pulverization. Because the problems of low crushing efficiency, softening, loss of volatile components, oxidation and the like exist in normal-temperature crushing, the invention adopts a low-temperature crushing technology to avoid the defects, keeps the effective components and components of the medicine unchanged and simultaneously improves the use quality and efficiency of the material.
2. Selection of raw material feeding mode
A Chinese medicine for treating lung cancer is prepared from Chinese-medicinal materials through pulverizing, decocting in water and extracting. According to the weight of the finished concentrated paste in different feeding modes, proper conditions are selected, and experimental results are shown as follows.
TABLE 2 influence of different feeding modes on the product
The first method comprises the following steps: directly adding the medicinal powder into cold water, heating, standing, and extracting.
And the second method comprises the following steps: discharging water from the tank, adding the medicinal powder into water in a container, stirring, standing, soaking for a certain time, and heating and extracting the medicinal liquid in a multifunctional extraction tank.
And (4) conclusion: from experimental results, in the first feeding mode, the amount of the concentrated extract of the extracting solution is low, and the extracting solution is not sufficient probably because the medicinal powder is agglomerated after absorbing water and water cannot sufficiently infiltrate into the inside. In the second mode, the quantity of the concentrated extract of the extracting solution is obviously increased, and the effective substance components are increased. Therefore, the mode of extraction after soaking is selected for feeding production.
According to the invention, by comparing two extraction modes of bulk decoction and pack decoction, the crushed medicinal materials are wrapped by a filter cloth and then soaked, and are decocted by adding water. The experimental results are shown below.
TABLE 3 Effect of different ways of decoction on the products
| Experimental number | 1 | 2 |
| Amount of prescription | 20kg | 20kg |
| Extraction method | Decocting in water to obtain decoction | Decocting in bag to obtain decoction |
| Relative density of final product | 1.014 | 1.014 |
| pH value of finished product | 5.61 | 5.60 |
| Content of finished product | 4.0mg/10ml | 4.1mg/10ml |
| Concentrated extract weight | 23.0kg | 23.8kg |
| Status of state | The extractive solution is viscous and not easy to filter | The extract is clear and easy to filter |
The first method comprises the following steps: adding the pulverized medicinal materials into water, stirring, standing, soaking for a certain time, and extracting with heating in a multifunctional extraction tank.
And the second method comprises the following steps: wrapping the pulverized medicinal materials with filter cloth, standing, soaking for a fixed time, and heating and extracting in a multifunctional extraction tank.
And (4) conclusion: from experimental results, the amount of concentrated extract of the extract and the content of active substances are slightly higher by adopting filter cloth package decoction extraction. After the product is subjected to bulk decoction and extraction, the soup is viscous, and the gauze bag is used for decoction, so that mucus can be prevented from permeating out, the soup is clear, and the next filtering and concentrating operation is facilitated. Therefore, the extraction method is comprehensively considered and selected.
3. Three-phase separation process
After the crude powder of the medicine is extracted and concentrated, water is added, an obvious amount of oily matter is obtained, the yellow oily matter is yellow and is slightly sticky, the oily matter cannot be intercepted by common filtration, the appearance state of a finished product is seriously influenced, and the turbid product is not clear. Therefore, a butterfly separator is adopted, a three-phase separation (liquid-solid) process is added, the adjusting speed is 50-150L/h, the temperature is 20-30 ℃, the pressure of a material inlet is 0.05-0.1mpa, the pressure of a material outlet is 0.05-0.3 mpa, and the experimental result is as follows:
TABLE 4 results of three-phase separation experiments
| Experimental number | Relative density | pH | Content (mg/10ml) (Rg1+ Re) |
| 1 | 1.014 | 5.6 | 4.0 |
| 2 | 1.011 | 6.0 | 3.9 |
And (4) conclusion: the quality indexes of the two batches of samples meet the quality standard. Through adopting the three-phase separation, not only stably get rid of oily composition, cleared away more tiny particle solid residue moreover, alleviateed subsequent filtration burden greatly, increased the filter speed.
4. Ultrafiltration process
The coarse powder extract is subjected to three-phase separation (liquid-solid) to obtain heavy phase liquid, and the heavy phase liquid is filtered by a microfiltration machine (the aperture of a microfiltration membrane is 0.45 μm, the working pressure is 0.10Mpa, the flow rate is 10t/h, and the temperature is 40 ℃) to obtain light yellow clear transparent liquid. And (5) standby.
And (3) taking the filtrate, respectively carrying out membrane separation and filtration on the filtrate through 10kDa, 30kDa, 50kDa, 80kDa and 100kDa hollow fiber ceramic membranes (transmembrane pressure difference of 0.35mpa, flow rate of 2.0m/s and temperature of 70 ℃), and collecting the filtrate. And (4) measuring the content of active ingredients in the liquid medicine after the membrane separation with different cut-off molecular weights.
TABLE 5 influence of different cut-off molecular weights on the liquid medicine after membrane separation
And (4) conclusion: from the above results, it can be seen that the solid content in the liquid medicine gradually increases with the increase of the molecular weight cut-off, but the content of ginsenoside Rg1 and ginsenoside Re in the sample does not change much, which indicates that most of the impurities in the solution are removed after membrane separation. As can be seen from the table, when the cut-off molecular weight is less than 30kDa, the content of active ingredients is reduced more, the cut-off molecular weight is 100kDa, and the solid content is not much different from that of the control group, so that the hollow fiber ceramic membrane with the cut-off molecular weight of 30kDa-80kDa is selected for ultrafiltration. Through the ultrafiltration process, clear and transparent liquid is obtained, macromolecular impurities such as microorganisms and proteins in the solution are removed, and the quality and the stability of the product are greatly improved. Solves the problems of turbidity and easy precipitation of the liquid medicine in the prior art, optimizes the process of the product and improves the taste of the product.
Example 7 quality control method
1. Content determination method of traditional Chinese medicine oral liquid for treating lung cancer
Preparation of control solutions: accurately weighing appropriate amount of ginsenoside Rg1 and ginsenoside Re reference substances, adding methanol to prepare solution containing ginsenoside Rg10.5mg and ginsenoside Re0.4mg per 1ml, and shaking up to obtain the final product.
Preparation of a test solution: precisely measuring 20ml of the prepared traditional Chinese medicine oral liquid, placing the traditional Chinese medicine oral liquid in a separating funnel, adding 10ml of water, extracting with trichloromethane for 2 times, 10ml each time, discarding the trichloromethane liquid, extracting the water solution with saturated n-butyl alcohol for 4 times, 25ml each time, performing ultrasonic treatment for 60min, filtering, drying the n-butyl alcohol liquid, adding methanol into residues for dissolving, transferring the residues to a 5ml measuring flask, adding methanol to scale, and shaking up to obtain the traditional Chinese medicine oral liquid.
And (3) determination: sucking 10ul of each of the two reference substance solutions and the sample solution, injecting into a liquid chromatograph, and measuring under the following chromatographic conditions:
octadecylsilane chemically bonded silica is used as a filling agent; acetonitrile-0.05% phosphoric acid solution (99:400) is used as a mobile phase; the detection wavelength was 203 mm. The number of theoretical plates is not less than 2500 calculated according to the peak of ginsenoside Re.
The product contains ginsenoside Rg1(C42H72O14) and ginsenoside Re (C48H82O18) in an amount of not less than 2.5mg per 10 ml.
2. Ultrasonic treatment method
In the preparation of the test solution, the aqueous solution was extracted with saturated n-butanol 4 times. The invention compares different processing methods of n-butanol extraction at the same time, and the experimental result is as follows,
TABLE 6 results of sonication experiments
And (4) conclusion: through comparison of experimental results, ultrasonic treatment is adopted, the method improves the yield of the ginsenoside and ensures the inspection accuracy of products.
3. Identification of traditional Chinese medicine oral liquid for treating lung cancer
The thin-layer identification is carried out on ginsenoside Re which is a marked component of ginseng, and the method comprises the following steps:
preparation of a test solution: taking 10ml of the prepared traditional Chinese medicine oral liquid, adding 10ml of water, placing in a separating funnel, extracting with chloroform for 2 times, 10ml each time, discarding chloroform solution, extracting the aqueous solution with water saturated n-butanol for 2 times, 30ml each time, combining n-butanol solution, adding ammonia test solution 30ml, shaking uniformly, standing for layering, collecting n-butanol solution, washing with water for 2 times, 40ml each time, discarding water solution, evaporating n-butanol solution to dryness, and adding methanol 1ml to the residue to dissolve to obtain a sample solution.
Preparation of control solutions: and adding methanol into ginsenoside Re reference substance to obtain 2ml solution per 1ml as reference substance solution.
The identification method comprises the following steps: and performing thin layer chromatography test, sucking the above two solutions 5ul, respectively dropping on the same silica gel G thin layer plate, developing with chloroform-ethyl acetate-methanol-water (15: 40: 22: 10) lower layer solution at 10 deg.C or below as developing agent, taking out, air drying, spraying 10% sulphuric acid ethanol solution, heating at 105 deg.C until the spots are clearly developed, and respectively inspecting under sunlight and ultraviolet light (365 nm). In the chromatogram of the test solution, spots or glowworm spots of the same color are located at positions corresponding to those of the chromatogram of the control solution.
The method for identifying the marker component of the coix seed, namely the glycerol trioleate, comprises the following steps:
preparation of control solutions: taking 10mg of triolein reference substance, precisely weighing, placing in a 10mL measuring flask, and adding petroleum ether to prepare 1mL solution containing 1mg of triolein.
Preparation of a test solution: pulverizing Coicis semen sample, weighing 1g powder, adding 10mL petroleum ether, ultrasonic treating for 30min, filtering, evaporating filtrate, and dissolving residue with 1mL petroleum ether to obtain Coicis semen reference solution.
Preparing a reference medicinal material solution: precisely weighing semen Coicis reference 1g, adding petroleum ether 10mL, performing ultrasonic treatment for 30min, filtering, evaporating filtrate, and dissolving residue with petroleum ether 1mL to obtain sample solution.
The identification method comprises the following steps: thin layer chromatography is used. Selecting silica gel G as stationary phase, using 0.5% sodium carboxymethyl cellulose solution as binder, respectively sucking 10L of glyceryl trioleate reference substance solution, test sample solution, and reference medicinal material solution, dropping on silica gel G plate, developing to 15cm with petroleum ether-ethyl acetate-glacial acetic acid (25: 5: 1) as developing agent, taking out, air drying, and spraying with 0.5% vanillin-concentrated sulfuric acid ethanol solution. Heating at 105 deg.C for 5min, viewing under ultraviolet lamp (365nm), wherein the spots are clearly visible, and the color spectrums of Coicis semen sample, reference substance and reference medicinal material are at corresponding positions, and show the same fluorescence spots.
EXAMPLE 8 clinical trial
One, general data
60 lung cancer patients who are collected at the end of 2018, 7 and 2019, 7 and 20 lung cancer patients are randomly divided into a control group and an experimental group, wherein the lung cancer patients are respectively 30 lung cancer patients. 20 male cases and 10 female cases in the control group, wherein the age is 40-75 years old; the experimental group comprises 18 men and 12 women, and the age is 40-77 years.
Second, Experimental methods
In the control group, the patients were treated with conventional chemotherapy, and the experimental group was administered with 1 (10ml) oral liquid of the Chinese medicinal composition prepared in example 1 on the basis of conventional chemotherapy, 3 times a day, and orally. Two groups extracted cases by random principle. Two groups are one treatment course per month, and 2 treatment courses are observed.
Third, observe the index
The total effective rate and the adverse reaction rate of the two groups of treatments are observed and compared, and the clinical effective rate of the treatment is evaluated according to the evaluation standard specified by WTO, namely, the total effective rate, the partial effective rate, the stability and the progress are completely relieved, partially relieved and stabilized.
Total effective rate is complete remission rate + partial remission rate
Fourth, observe the results
The results are shown in tables 7 and 8:
TABLE 7 comparison of the total effective rates of the two groups of patients
| Group of | Number of examples | Complete relief | Partial relief | Stabilization | Progress of the development | High efficiency |
| Experimental group | 30 | 11 | 10 | 6 | 3 | 70％ |
| Control group | 30 | 8 | 7 | 9 | 6 | 50％ |
TABLE 8 comparison of adverse reaction incidence rates in two groups of patients
| Group of | Number of examples | Leukocyte reduction | Liver function abnormality | Nausea and vomiting | Incidence rate |
| Experimental group | 30 | 0 | 0 | 0 | 0％ |
| Control group | 30 | 1 | 2 | 1 | 3％ |
And (4) conclusion: the clinical effective rate of the experimental group is obviously higher than that of the control group, and no toxic or side effect and adverse reaction are found in the treatment. The product of the invention is a better medicament for adjuvant therapy of lung cancer.
Example 9 human body test
First, subject enrollment criteria: the BMI of an adult is more than or equal to 30 in a simple obese population, or the total fat percentage reaches more than 25 percent for men and more than 30 percent for women. Exclusion criteria: (1) patients with serious diseases of heart, liver, kidney and hemopoietic system, and psychosis; (2) taking medicines or foods related to the tested function in a short period of time to influence the judgment of the result; (3) if the test sample is not eaten according to the regulations, the efficacy or the safety judgment cannot be judged.
II, a test method: 60 subjects are included, 30 subjects are fed in the test group, 30 subjects are controlled in the control group, and the examinations of blood routine, urine routine, stool routine, liver and kidney functions, chest penetration, electrocardiogram and the like of the subjects before the test are all within a normal range, and the age, sex, weight losing time, body weight index and percentage index of the patients in the former two groups are not obviously different (P is more than 0.05); the Chinese medicinal oral liquid prepared in example 1 was administered to the test group 1 (10ml) each time, 3 times a day, orally for 60 days, and the control group was administered to the blank control. The feeding trial was performed according to the double-blind method.
TABLE 9 weight changes before and after two groups of test diets
| Group of | Number of examples | Before tasting (kg) | After tasting (kg) |
| Test food group | 30 | 86.56±8.19 | 79.60±7.78 |
| Control group | 30 | 84.78±10.79 | 84.65±9.79 |
And (4) test conclusion: clinical tests show that the preparation has good weight reducing effect and can be clinically applied to obese patients.
Claims (10)
1. A preparation method of a traditional Chinese medicine oral liquid for treating lung cancer is characterized by comprising the following steps:
(1) low-temperature crushing and weighing:
pulverizing ginseng and coix seeds into coarse powder at a low temperature of 0-15 ℃, sieving the coarse powder by a 20-100-mesh sieve, and weighing the coarse powder according to the proportion of 0.5-3 parts by weight of ginseng and 1-9 parts by weight of coix seeds;
(2) decocting and filtering:
wrapping the pulverized medicinal materials with filter cloth, soaking in water, decocting with water twice, the first time with 11-13 times of water for 1-2 hr, the second time with 7-9 times of water for 0.5-1.5 hr, mixing decoctions, and filtering;
(3) concentrating and recovering ethanol:
concentrating the filtrate to relative density of 1.18-1.22 at 50 deg.C, adding 2 times volume of ethanol, standing for 10-12 hr, collecting supernatant, and recovering ethanol until no ethanol smell exists;
(4) three-phase separation:
adding water to the prescribed amount, performing three-phase separation by using a three-phase butterfly separator, and taking heavy-phase liquid for later use;
(5) and (3) filtering:
filtering the heavy phase liquid by using a micro-filter, and ultrafiltering the filtrate by using a hollow fiber ceramic membrane with the molecular weight cutoff of 30-80 kDa, wherein the filtrate is for later use;
(6) filling and sealing, and sterilizing:
and (5) taking the filtrate obtained in the step (5), filling and sealing, and sterilizing to obtain the traditional Chinese medicine.
2. The preparation method according to claim 1, wherein the crude powder is prepared by weighing 1 part by weight of ginseng and 4-6 parts by weight of coix seed, preferably 1 part by weight of ginseng and 5 parts by weight of coix seed.
3. The preparation method according to claim 1, wherein the production capacity of the three-phase butterfly separator is 50-150L/h, the temperature is 20-30 ℃, the pressure at the material inlet is 0-0.1MPa, and the pressure at the material outlet is 0-0.3 MPa.
4. The preparation method of claim 1, wherein the microfiltration membrane of the microfiltration machine has a pore size of 0.2 to 1.0 μm, a working pressure of 0.10 to 0.6Mpa, a flow rate of 5 to 30t/h and a temperature of 20 to 60 ℃.
5. The process according to claim 1, wherein the ultrafiltration has a transmembrane pressure difference of 0.1 to 0.5mpa, a flow rate of 1.0 to 5.0m/s and a temperature of 50 to 80 ℃.
6. The preparation method according to any one of claims 1 to 5, further comprising a step of performing quality control on the prepared Chinese medicinal oral liquid, comprising:
(1) preparation of control solutions:
accurately weighing appropriate amount of ginsenoside Rg1 and ginsenoside Re reference substances, adding methanol to obtain reference substance solution containing ginsenoside Rg10.5mg or ginsenoside Re0.4mg per 1ml, and shaking;
(2) preparation of a test solution:
precisely measuring 20ml of the prepared traditional Chinese medicine oral liquid, placing the oral liquid in a split-flow funnel, adding 10ml of water, extracting with chloroform for 2 times, 10ml each time, discarding chloroform solution, extracting the water solution with saturated n-butanol for 4 times, 25ml each time, performing ultrasonic treatment for 60min, filtering, evaporating n-butanol solution to dryness, dissolving the residue with methanol, transferring the dissolved residue to a 5ml measuring flask, adding methanol to scale, and shaking up to obtain the traditional Chinese medicine oral liquid;
(3) and (3) determination:
respectively sucking 10ul of each of the two reference substance solutions and the test sample solution, injecting into a liquid chromatograph, and measuring under the following chromatographic conditions:
filling agent: octadecylsilane chemically bonded silica;
mobile phase: the volume ratio of 99:400 acetonitrile-0.05% phosphoric acid solution as mobile phase;
detection wavelength: 200-250 nm;
the number of theoretical plates: calculated according to the peak of ginsenoside Re, should not be lower than 2500.
7. The method according to claim 6, wherein the detection wavelength in the step (3) is 203 nm.
8. The method of any one of claims 1 to 7, further comprising the step of identifying the prepared oral liquid of traditional Chinese medicine, comprising:
(1) the thin-layer identification of ginsenoside Re as the marker component of ginseng comprises the following steps:
1) preparing a test solution:
taking 10ml of the prepared traditional Chinese medicine oral liquid, adding 10ml of water, placing in a separating funnel, extracting with chloroform for 2 times, 10ml each time, discarding chloroform solution, extracting aqueous solution with water saturated n-butanol for 2 times, 30ml each time, combining n-butanol solution, adding ammonia test solution 30ml, shaking uniformly, standing for layering, collecting n-butanol solution, washing with water for 2 times, 40ml each time, discarding water solution, evaporating n-butanol solution to dryness, and adding methanol 1ml to residue for dissolving to obtain sample solution;
2) preparation of a reference substance: adding methanol into ginsenoside Re reference substance to obtain 2ml solution per 1ml as reference substance solution;
3) the identification method comprises the following steps:
according to the thin layer chromatography test, 5ul of each of the test solution and the reference solution is sucked and respectively spotted on the same silica gel G thin layer plate according to the volume ratio of 15: 40: 22: 10 chloroform-ethyl acetate-methanol-aqueous solution, taking the lower layer solution placed below 10 ℃ as a developing agent, developing, taking out, airing, spraying 10% sulfuric acid ethanol solution, heating at 105 ℃ until the color of the spots is clearly developed, respectively inspecting under sunlight and 365nm ultraviolet light, and displaying the spots or glowworm spots with the same color in the chromatogram of the test sample at the positions corresponding to the chromatogram of the reference sample;
(2) the method for identifying the marker component of the coix seed, namely the glycerol trioleate, comprises the following steps:
1) preparation of control solutions:
taking 10mg of triolein reference substance, precisely weighing, placing in a 10mL measuring flask, and adding petroleum ether to prepare 1mL solution containing 1mg of triolein;
2) preparation of a test solution:
taking a coix seed raw material for preparing the traditional Chinese medicine oral liquid, crushing, weighing 1g of powder, adding 10mL of petroleum ether, carrying out ultrasonic treatment for 30min, filtering, evaporating filtrate to dryness, and dissolving residues in 1mL of petroleum ether to obtain a sample solution;
3) preparing a reference medicinal material solution:
precisely weighing semen Coicis reference material 1g, adding petroleum ether 10mL, ultrasonic treating for 30min, filtering, evaporating filtrate, dissolving residue with petroleum ether 1mL to obtain semen Coicis reference material solution;
4) the identification method comprises the following steps:
adopting thin layer chromatography, selecting silica gel G as stationary phase, using 0.5% w/w sodium carboxymethylcellulose solution as adhesive, respectively absorbing 10uL of each of glyceryl trioleate reference solution, test sample solution and reference medicinal material solution, dropping on silica gel G plate, and dispensing with a volume ratio of 25: 5: 1, developing to 15cm, taking out, air drying, spraying 0.5% vanillin-98% concentrated sulfuric acid ethanol solution, heating at 105 deg.C for 5min, and inspecting under 365nm ultraviolet lamp to obtain clear spots, wherein the chromatogram of Coicis semen sample, reference substance and reference material shows the same fluorescent spots.
9. A Chinese medicinal oral liquid prepared according to the method of any one of claims 1 to 8.
10. Use of the Chinese medicinal oral liquid according to claim 9 for preparing a medicament for treating lung cancer and/or reducing weight.
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| 胡静波等: "三相分离技术提取大豆油", 《河南工业大学学报》, vol. 30, no. 04, 31 August 2009 (2009-08-31), pages 32 - 35 * |
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Application publication date: 20210907 |