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CN119198998A - Process for identifying main active ingredients of Naomaili granules - Google Patents

Process for identifying main active ingredients of Naomaili granules Download PDF

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Publication number
CN119198998A
CN119198998A CN202310760464.1A CN202310760464A CN119198998A CN 119198998 A CN119198998 A CN 119198998A CN 202310760464 A CN202310760464 A CN 202310760464A CN 119198998 A CN119198998 A CN 119198998A
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solution
naomaili
peak
granules
reference substance
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陈冠良
熊锴
王超磊
曹红光
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Jiangsu Carephar Pharmaceutical Co ltd
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Jiangsu Carephar Pharmaceutical Co ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/90Plate chromatography, e.g. thin layer or paper chromatography

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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Abstract

本发明公开了一种鉴别脑脉利颗粒主要有效成分的工艺,取脑脉利颗粒1g,研细,加70%乙醇25ml,超声处理30分钟,滤过,滤液蒸干,残渣加无水乙醇1ml使溶解,作为供试品溶液。本发明采用一种极性相近的展开剂,既避免了试剂对人体、环境的危害,又对达到了检测目标物能够较好分离检出的效果。

The invention discloses a process for identifying the main active ingredients of Naomaili granules, wherein 1g of Naomaili granules is taken, ground, 25ml of 70% ethanol is added, ultrasonic treatment is performed for 30 minutes, filtration is performed, the filtrate is evaporated to dryness, and 1ml of anhydrous ethanol is added to the residue to dissolve it as a test solution. The invention adopts a developing agent with similar polarity, which not only avoids the harm of the reagent to the human body and the environment, but also achieves the effect of better separation and detection of the detection target.

Description

Process for identifying main active ingredients of Naomaili granules
Technical Field
The invention belongs to the technical field of biological medicines, and particularly relates to a process for identifying main active ingredients of Naomaili granules.
Background
In recent years, the main population suffering from cerebral apoplexy is still middle-aged and elderly people, and the average age of onset of patients is about 65 years. However, with the aging of population and the acceleration of the urbanization process, lifestyle is continuously changing, and the number of people suffering from cerebrovascular diseases is continuously increasing and gradually showing a younger trend. Therefore, treatment of cerebral stroke, especially ischemic cerebral stroke, is not very slow.
According to the content of Chinese instructions 2018 for diagnosis and treatment of acute ischemic cerebral apoplexy, specific treatment schemes for acute ischemic cerebral apoplexy comprise cerebral blood circulation improvement, statin drugs, neuroprotection, hyperbaric oxygen treatment and sub-hypothermia treatment, and traditional medical therapies of Chinese patent medicines and acupuncture.
The ultra-early treatment of acute ischemic cerebral apoplexy mainly aims at realizing vascular recanalization, restoring blood circulation and rebuilding, and saving ischemic penumbra, but reperfusion injury, reocclusion and hemorrhagic transformation are common after vascular recanalization. The traditional Chinese medicine clinic considers that thrombolysis is a method of consuming qi and damaging blood, and the conditions after the early thrombolysis are all marked by qi deficiency and blood stasis, and the symptoms are marked by excess.
Therefore, the main treatment strategy in traditional Chinese medicine is to benefit qi and nourish blood, promote blood circulation and remove meridian obstruction as an auxiliary, treat both principal and secondary aspect of the disease, implement multi-way comprehensive protection on each component of the neurovascular unit in each stage of ischemia/reperfusion, and further improve the treatment effect of ischemic cerebral apoplexy. The Naomaili granule is a unique traditional Chinese medicine oral preparation produced by adopting a modern pharmaceutical technology on the basis of a classical formula of 'Buyang Huanwu Tang' by Jiangsu Ke Feiping medical stock, has the action characteristics of multiple targets and multiple ways of traditional Chinese medicines, generates comprehensive treatment effect, and is used for treating ischemic cerebral apoplexy.
However, in the original execution standard of Naomaili granules, the developing agent for identifying the main active ingredients of the finished granules contains benzene, so that the developing agent has high toxicity, strong harm to the body of a tester and serious environmental pollution, and therefore, the developing agent with similar polarity is developed, so that the harm of the reagent to the human body and the environment is avoided, and the effect of better separating and detecting the detection target object is achieved.
Disclosure of Invention
The invention aims to provide a process for identifying main active ingredients of Naomaili particles, which solves the problems in the prior art, adopts a developing agent with similar polarity, avoids the harm of the reagent to human bodies and the environment, and achieves the effect of better separating and detecting the detection target objects.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a process for identifying main active ingredients of Naomaili granules comprises the following steps:
taking 1g of Naomaili granules, grinding, adding 25ml of 70% ethanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, and adding 1ml of absolute ethanol into residues to dissolve the residues to obtain a sample solution;
adding herba Leonuri control 1g into water 50ml, boiling for 30 min, filtering, evaporating filtrate to dryness, adding 70% ethanol 25ml into the residue, and making into medicinal solution;
Taking a stachydrine hydrochloride reference substance, adding absolute ethyl alcohol to prepare a solution containing 1mg per lml as a reference substance solution;
performing thin layer chromatography test;
In the sample chromatogram, the spots with the same color are identified at the positions corresponding to the control chromatogram and the control chromatogram.
The thin layer chromatography test comprises the following specific steps:
According to the thin layer chromatography test, 8 μl of the sample solution is sucked, 10 μl of each of the control medicinal material solution and the control solution is respectively spotted on the same silica gel G thin layer plate, acetone-absolute ethyl alcohol-hydrochloric acid is used as developing agent, and the developing agent is developed, taken out, dried in the air, sprayed with the mixed solution of dilute bismuth potassium iodide test solution and ferric trichloride test solution, heated at 105 ℃ for 15 minutes, and inspected under sunlight.
The preparation method further comprises the steps of precisely sucking 1 mu l of each of the reference substance solution and the sample solution, injecting the sample solution into a liquid chromatograph for measurement to obtain 9 characteristic peaks in the sample chromatograph, corresponding to the retention time of the 9 characteristic peaks in the reference substance chromatograph of the reference medicinal material, taking the peak corresponding to the reference substance peak of leonurine hydrochloride as an S peak, and calculating the relative retention time of each characteristic peak and the S peak, wherein the relative retention time is within +8% Fan Yong of a specified value.
Compared with the prior art, the invention has the beneficial effects that:
The invention adopts the developing agent with similar polarity, thereby avoiding the harm of the reagent to human bodies and the environment and achieving the effect of better separating and detecting the detection target objects.
In the original execution standard of Naomaili granule, the content of the target compound is 'stachydrine hydrochloride', the detection method uses a lotus layer scanning method, the detection time is long, and the single-batch detection time is 2 days. In a newly developed high performance liquid chromatography-evaporative light scattering detector, an external standard two-point logarithmic method and a comprehensive methodology research is carried out on the novel method, the method has strong specificity and good durability, precision and accuracy. Meanwhile, the method has the characteristics of short time consumption, labor conservation, advanced method and the like.
(1) The dry granulating process is more matched with the characteristics of the product, and after the dry granulating process is changed into the dry granulating process, the steps of drying and total leakage in the original wet granulating process can be removed, the production efficiency of the product is improved, the production process is easier to control, and the post operation is simpler;
(2) The dry granulating process can reduce the production energy consumption, save energy and reduce emission, greatly reduce the production time from granulating to obtaining the total mixed intermediate, reduce the consumption of a public system, fuel energy consumption and the like from 24 hours/batch of the wet process to 8 hours/batch, greatly reduce the labor hour of personnel, and reduce the production cost to a certain extent;
(3) Compared with wet granulation, the yield of dry granulation can be higher, so the yield of the dry granulation process is improved from 85% of the wet granulation process to 90%.
(4) The product has high crude drug content, and daily dosage is 106.8g of crude drug, and single dosage is about 20 times of thousand similar products. The quality of the preparation is ensured by adopting different extraction processes and qualitative and quantitative analysis of 8 main effective components.
(5) In the production process of Naomaili granules, the 11 medicinal materials are extracted, inclusion complex and dry extract are fully and uniformly mixed, and then the Naomaili granules are prepared by an advanced dry granulation process, so that the active ingredients are reserved to the greatest extent.
(6) In the aspect of quality control, an internal control standard higher than that of Chinese pharmacopoeia is formulated, and the effective components of 8 medicinal materials in the formula are quantitatively and qualitatively checked, so that the quality control of Naomaili granules is ensured, and the curative effect is stable.
Drawings
FIG. 1 is a comparative characteristic spectrum of leonurine hydrochloride.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Embodiment one.
Taking 1g of Naomaili granules, grinding, adding 25ml of 70% ethanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, and adding 1ml of absolute ethanol into residues to dissolve the residues to obtain a sample solution;
adding herba Leonuri control 1g into water 50ml, boiling for 30 min, filtering, evaporating filtrate to dryness, adding 70% ethanol 25ml into the residue, and making into medicinal solution;
Taking a stachydrine hydrochloride reference substance, adding absolute ethyl alcohol to prepare a solution containing 1mg per lml as a reference substance solution;
according to thin layer chromatography (rule 0502 of Chinese pharmacopoeia 2020 edition), sucking 8 μl of sample solution, 10 μl of control medicinal solution and 10 μl of control solution, respectively spotting on the same silica gel G thin layer plate, spreading with acetone-anhydrous alcohol-hydrochloric acid (10:6:1) as developing agent, taking out, air drying, spraying mixed solution of dilute bismuth potassium iodide solution-ferric trichloride solution (10:1), heating at 105deg.C for 15 min, and inspecting in sunlight.
In the sample chromatogram, the spots with the same color are identified at the positions corresponding to the control chromatogram and the control chromatogram.
Preparing reference solution by placing 1.5g of herba Leonuri control into conical flask with plug, adding 25ml of water, boiling for 30 min, filtering, adding 20ml of water into the residue, boiling for 20min, filtering, mixing filtrates, evaporating under reduced pressure, adding 25ml of 50% methanol into the residue, ultrasonic treating (power 250W, frequency 40 kHz) for 30 min, filtering, and collecting filtrate as reference solution. And taking the leonurine hydrochloride reference substance solution under the item [ content measurement ] as a reference substance solution of the reference substance.
The preparation of the test solution is carried out under the same condition (content measurement) as that of leonurine hydrochloride.
The measuring method comprises respectively precisely sucking 1 μl of reference solution and 1 μl of sample solution, and injecting into a liquid chromatograph for measurement to obtain 9 characteristic peaks in the sample chromatogram, corresponding to 9 characteristic peaks in the reference chromatogram of the reference medicinal material, and corresponding to the reference peak of leonurine hydrochloride as S peak, and calculating the relative retention time of each characteristic peak and S peak, wherein the relative retention time is within +8% Fan Yong of the specified value. The predetermined values were 039 (peak 1), 0.9 (peak 2), 0.57 (peak 3), 0.74 (peak 4), 1.05 (peak 6), 1.50 (peak 7), 1.66 (peak 8), and 1.72 (peak 9).
Checking that the prescription (the rule 0104 of the edition of Chinese pharmacopoeia 2020) of the granule should be met.
The extract is obtained by hot dipping under alcohol soluble extract assay (2201) in Chinese pharmacopoeia 2020 edition, and using ethanol as solvent, and is not less than 19.0%.
The content measurement comprises measuring leonurine hydrochloride by high performance liquid chromatography (China Pharmacopeia 2020 edition general rule 0512).
Chromatography conditions and system applicability test were carried out using octadecylsilane chemically bonded silica as filler (column length of 100mm, column inner diameter of 2.1mm, particle diameter of 1.7 m), nitrile as mobile phase A,0.1% phosphoric acid solution as mobile phase B, gradient elution was carried out as specified in the following table at a flow rate of 0.4 ml/min, column temperature of 35C and detection wavelength of 277nm. The theoretical plate number is not less than 6000 according to the leonurine hydrochloride peak.
Table 1. Chromatographic conditions and system suitability test data table.
Preparing reference solution, precisely weighing, and adding 50% methanol to obtain solution containing 40ug per 1 ml.
The preparation of the sample solution comprises taking a proper amount of the sample, grinding, taking about 0.2g, precisely weighing, placing into a conical flask with a plug, finely adding 25ml of 50% methanol, sealing, weighing, performing ultrasonic treatment (power is 250W, frequency is 40 kHz) for 30 minutes, taking out, cooling, weighing again, supplementing the lost weight with 50% methanol, shaking, filtering, and taking the subsequent filtrate.
The measurement method comprises precisely sucking 1ul of each of the reference solution and the sample solution, and injecting into a liquid chromatograph for measurement.
The content of leonurine hydrochloride (C14H 21 O5N3.HCl) in each 1g of the product is 1.5 mg-4.9 mg.
Embodiment two.
The stachydrine hydrochloride is determined by high performance liquid chromatography.
Chromatographic conditions and System applicability test by using propyl amide bonded silica gel as filler, acetonitrile-0.2% glacial acetic acid solution (80:20) as mobile phase, detection with evaporative light scattering detector, flow rate of 1.2ml per minute, and column temperature of 40deg.C. The theoretical plate number is calculated according to hydrochloric acid water Su Jianfeng and is not lower than 6000.
Preparation of reference solution A proper amount of stachydrine hydrochloride reference is taken, precisely weighed, and methanol is added to prepare a solution containing 0.3mg per 1 ml.
The preparation of the sample solution comprises grinding proper amount of the sample, taking about 0.2g, precisely weighing, placing into a conical flask with a plug, precisely adding 20ml of methanol, weighing, performing ultrasonic treatment (power 250W, frequency 40 kHz) for 30 minutes, taking out, cooling, weighing again, supplementing the lost weight with methanol, shaking, filtering, and collecting the subsequent filtrate.
The measuring method comprises the steps of precisely sucking 10 mu l of reference substance solution and 15 mu l of sample solution, injecting 10-20 mu l of sample solution into a liquid chromatograph, measuring, and calculating by using an external standard two-point logarithmic equation.
The content of the stachydrine (CH 1NO2. HCl) in each 1g of the product is 18.8 mg-60.0 mg.
Each 1g of the formula granule is equivalent to 4.5-6.5g of decoction pieces, and the dosage of each dose is equivalent to about 20 times of thousands of similar products.
The brain-meridian-benefiting product comprises herba Leonuri, notoginseng radix, radix astragali, curcuma rhizome, rhizoma Ligustici Chuanxiong, carthami flos, saviae Miltiorrhizae radix, radix Paeoniae Rubra, radix Angelicae sinensis, radix Paeoniae alba and radix Cyathulae as main ingredients.
The characteristics are that the product is brown granule, has slight smell and bitter taste.
Has the functions of promoting blood circulation to disperse blood clots, invigorating vital energy and dredging meridian. Can be used for treating apoplexy due to qi deficiency and blood stasis (cerebral infarction) with symptoms of hemiplegia, hemianesthesia, facial distortion, and slurred speech.
The main components of the finished product are as follows:
1. Motherwort:
The product is fresh or dried aerial parts of herba Leonuri Leonurus japonicus Houtt of Labiatae. Fresh product is picked and cut from spring seedling stage to early stage of early summer flower, and dried product is picked and cut, dried or cut and dried when stem and leaf are luxuriant and flowers are not opened or are initially opened.
The characteristics are that the fresh motherwort has no stem in the seedling stage, the basal leaves are round and heart-shaped, 5-9 shallow cracks are formed, and each crack has 2-3 blunt teeth. The stem at the early stage of flowers is in a square column shape, the upper part is multi-branched, four sides are concave to form longitudinal grooves, the length is 30-60 cm, the diameter is 0.2-0.5cm, the surface is dark green, the quality is fresh and tender, and the middle part of the cross section is provided with marrow. She Jiaohu are green, fresh and tender, and the lower part is cracked into palm shape, the upper part She Yuzhuang is cracked deeply or shallowly into 3 pieces, and the whole edge of the split piece is provided with a few sawteeth. Light smell and slightly bitter taste.
The surface of the stem of motherwort is grey green or yellow green, the body is light, the quality is tough, and the middle part of the section is provided with marrow. The leaves are gray green, and are more shrunken and crushed, and are easy to fall off. Axillary growth of the clitocybe maxima, light purple floret, cylindrical calyx and two lips of corolla.
The nature and flavor are bitter and pungent and slightly cold. Enter liver, pericardium and bladder meridians.
Has the functions of promoting blood circulation, regulating menstruation, promoting urination, reducing swelling, clearing away heat and toxic material. Can be used for treating menoxenia, dysmenorrhea, amenorrhea, lochiorrhea, edema, oliguria, and pyocutaneous disease.
2. Pseudo-ginseng:
The product is dried root and rhizome of Panax notoginseng Panax notoginseng (Burk.) F.H.Chen. Digging before autumn flowers, cleaning, separating main root, branch root and rhizome, and drying. The root is called "rib" and the rhizome is called "cut".
The main root is conical or cylindrical, and has a length of 1-6 cm and a diameter of 1-4 cm. The surface is grey brown or grey yellow, and has intermittent longitudinal wrinkles and branch root marks. The top end is provided with stem mark, and the periphery is provided with tumor-shaped protrusions. The weight is firm, the section is gray green, yellow green or gray white, and the wood parts are slightly arranged in a radial shape. Light smell, bitter and sweet taste.
The ribs are cylindrical or conical, the length is 2-6 cm, the diameter of the upper end is about 0.8cm, and the diameter of the lower end is about 0.3cm.
The shearing mouth is in an irregular shrinkage block shape or a strip shape, the surface is provided with a plurality of obvious stem marks and ring patterns, the center of the section is gray or white, and the edges are dark green or gray.
The nature and flavor are sweet, slightly bitter and warm. Enter liver and stomach meridians.
Has the functions of eliminating blood stasis, stopping bleeding, eliminating swelling and relieving pain. Can be used for treating hemoptysis, hematemesis, epistaxis, hematochezia, metrorrhagia, traumatic hemorrhage, thoracico-abdominal pain, and traumatic injury.
3. Radix astragali:
the product is dried root of Astragalus mongholicus Astragalus membranaceus (Fisch.) bge. Var. Mongholicus (bge.) Hsiao or Astragalus membranaceus Astragalus membranaceus (Fisch.) bge. Collected in spring and autumn, removed fibrous root and root head, and dried in the sun.
The product is cylindrical, has branches, and has a thicker upper end, a length of 30-90 cm and a diameter of 1-3.5 cm. The surface is light brown yellow or light brown, and has irregular longitudinal wrinkles or longitudinal furrows. Hard and tough, not easy to break, strong in section fiber, and powder-developing, yellowish white in skin, pale yellow in wood, radial textures and cracks, and dead and dark brown or hollow in old root center. Slight smell, slightly sweet taste, slightly beany flavor after chewing.
The nature and flavor are sweet and slightly warm. Enter lung and spleen meridians.
Has the functions and the main functions of tonifying qi and yang, strengthening exterior and arresting sweating, inducing diuresis and relieving edema, promoting the production of body fluid and nourishing blood, promoting the circulation of qi and relieving arthralgia, expelling toxin and expelling pus, healing sore and promoting tissue regeneration. Can be used for treating qi deficiency, debilitation, loose stool, depression of middle-jiao, chronic diarrhea, rectocele, hematochezia, metrorrhagia, spontaneous perspiration, qi deficiency, edema, internal heat, diabetes, blood deficiency, sallow complexion, hemiplegia, arthralgia, numbness, carbuncle, ulcer, and chronic ulcer.
4. Turmeric:
The product is dried rhizome of Curcuma rhizome Curcuma Longa L of Zingiberaceae. Digging when stem and leaf wilt in winter, cleaning, boiling or steaming until the stem and leaf is transparent, sun drying, and removing fibrous root.
The product is in an irregular oval shape, a cylindrical shape or a spindle shape, is often bent, has short fork-shaped branches, and has a length of 2-5 cm and a diameter of 1-3 cm. The surface is deep yellow and rough, has shrinkage textures and obvious links, and has round branch marks and fibrous root marks. Firm, not easy to break, brown to golden yellow cross section, cutin-like, wax-like luster, obvious ring lines of the endothelial layer, and scattered vascular bundles in dotted form. Specific smell, bitter and pungent taste.
The nature and flavor are pungent and bitter and warm. Enter spleen and liver meridians.
Has the functions and the main functions of breaking blood, promoting qi circulation, dredging channels and relieving pain. Can be used for treating chest and hypochondrium pain, chest pain, dysmenorrhea, amenorrhea, abdominal mass, rheumatic shoulder and arm pain, and traumatic injury.
5. Ligusticum wallichii:
The product is dried rhizome of Ligusticum chuanxiong Ligusticum chuanxiong Hort belonging to Umbelliferae. In summer, when the node discs on the stems are obvious and slightly purple, the node discs are dug, sediment is removed, and the node discs are dried after sun drying and fibrous roots are removed.
The character is that the product is an irregular nodular fist-shaped block with the diameter of 2-7 cm. The surface is grey brown or brown, rough and shrunk, the surface is provided with a plurality of parallel raised wheel nodes, the top end of the wheel node is provided with a concave similar circular stem mark, and the underside and the wheel nodes are provided with a plurality of small tumor-shaped root marks. Solid, not easy to break, yellow-white or grey-yellow in cross section, dispersed with yellow-brown oil chamber, and the layer ring is wave-shaped. Strong smell, bitter and pungent taste, slightly tingling and sweet taste.
The nature and flavor are pungent and warm. Enter liver, gallbladder and pericardium meridians.
Has the functions of promoting blood circulation, promoting qi circulation, dispelling wind and relieving pain. Can be used for treating chest pain, hypochondrium pain, traumatic injury, menoxenia, amenorrhea, dysmenorrhea, abdominal pain, headache, and rheumatalgia.
6. Safflower:
The product is dried flower of safflower Carthamus tinctorius L. The flowers are picked up in summer and dried in the shade or sun-dried when the flowers turn from yellow to red.
The character is that the product is a tubular flower without ovary, and the length is 1-2 cm. The surface is red-yellow or red. The crown cylinder is slender, the tip 5 is split, the split is in a narrow strip shape and is 5-8 mm long, the stamen 5 is formed by polymerizing anthers into a cylinder shape which is yellow and white, the column head is long and the top is slightly bifurcated. Soft in texture. Slightly fragrant and slightly bitter.
The nature and flavor are pungent and warm. It enters heart and liver meridians.
Has the functions and the main functions of promoting blood circulation, dredging channels, removing blood stasis and relieving pain. Can be used for treating amenorrhea, dysmenorrhea, lochia, abdominal mass, chest pain, abdominal pain due to blood stasis, thorny chest and hypochondrium, traumatic injury, and swelling and pain.
7. Root of red-rooted salvia:
The product is dry root and rhizome of Salvia Miltiorrhiza Salvia miltiorrhiza bge. Collected in spring and autumn, removed sediment, and dried.
The characteristic is that the rhizome of the product is short and thick, and the top end of the product sometimes remains the stem base. A plurality of branches, a long cylinder, a little bent, some branches and whisker-shaped thin roots, the length of which is 10-20 cm and the diameter of which is 0.3-1 cm. The surface is brownish red or dark brownish red, is rough and has longitudinal wrinkles. The outer skin of the old root is loose and has a plurality of purple-brown colors, and is often flaked. Hard and brittle, loose cross section, fissure or slightly flat and compact, brown red skin, grey yellow or purple brown wood, yellow white catheter bundle, and radial arrangement. Light smell, slightly bitter and astringent taste.
The cultivated product is thicker and has the diameter of 0.5-1.5 cm. The surface is reddish brown, has longitudinal wrinkles, and the crust is tightly attached and is not easy to peel off. Firm, flat and slightly keratotic.
The property and taste are bitter and slightly cold. It enters heart and liver meridians.
Has the functions of promoting blood circulation to disperse blood clots, dredging meridian, relieving pain, clearing away heart-fire, eliminating vexation, cooling blood and eliminating carbuncle. Can be used for treating chest pain, abdominal pain, hypochondriac pain, abdominal mass, pain due to pyretic arthralgia, vexation, insomnia, menoxenia, dysmenorrhea, amenorrhea, and pyocutaneous disease.
8. Radix paeoniae rubra:
The product is dried root of Paeonia lactiflora Paeonia lactiflora pall or Paeonia sicca VEITCHII LYNCH belonging to Ranunculaceae. Collected in spring and autumn, removed rhizome, fibrous root and sediment, and dried in the sun.
The product is cylindrical, slightly bent, 5-40 cm long and 0.5-3 cm in diameter. The surface is brown, rough, has longitudinal grooves and wrinkles, has fibrous root marks and transverse long skin hole-like protrusions, and has skin which is easy to fall off. Hard and brittle, easy to break, white or pink broken flour, narrow skin, obvious radial texture of wood and cracks. Slightly fragrant, slightly bitter, sour and astringent.
The property and taste are bitter and slightly cold. Enter liver meridian.
Has the functions of clearing heat, cooling blood, dispersing blood stasis and relieving pain. Can be used for treating heat-induced ying blood, toxic heat, speckle, hematemesis, epistaxis, conjunctival congestion, swelling and pain, liver Yu Xie pain, amenorrhea, dysmenorrhea, abdominal pain, traumatic injury, carbuncle, swelling and sore.
9. Chinese angelica root:
The product is dry root of Angelica sinensis ANGELICA SINENSIS (Oliv.) Diels belonging to Umbelliferae. Digging in autumn, removing fibrous root and silt, slightly evaporating water, bundling into small bundles, placing in a shed, and smoking with smoke and fire.
The product is cylindrical, and has 3-5 or more branches at the lower part and 15-25 cm long. The surface is light brown to tan, and has longitudinal wrinkles and transverse leather hole-like protrusions. The root head (return head) has a diameter of 1.5-4 cm, has annular lines, is round at the upper end, or has a plurality of obviously protruding rhizome marks, has purple or yellowish green stems and leaf sheath residues, has uneven surfaces of main roots (return bodies), has a diameter of 0.3-1 cm, and has thick upper parts and thin lower parts, multiple twists and few fibrous root marks. The soft wood has a yellow-white or light yellow brown cross section, thick skin, fissures and a plurality of brown punctiform secretion cavities, and lighter wood color, and forms a ring yellow brown. Has strong fragrance, sweet, pungent and slightly bitter.
The nature and flavor are sweet, pungent and warm. It enters liver, heart and spleen meridians.
Has the functions and the main functions of enriching and activating blood, regulating menstruation and relieving pain, and relaxing bowel. Can be used for treating sallow complexion due to blood deficiency, dizziness, palpitation, menoxenia, amenorrhea, dysmenorrhea, abdominal pain due to deficiency-cold, rheumatalgia, traumatic injury, carbuncle, skin ulcer, and constipation due to intestinal dryness. The wine angelica can promote blood circulation and promote menstruation. Can be used for treating amenorrhea dysmenorrhea, rheumatalgia, traumatic injury.
10. White peony root:
The product is dried root of Pall. Paeonia lactiflora Pall Paeonia lactiflora belonging to Ranunculaceae. Digging in summer and autumn Ji, cleaning, removing head, tail and root, decocting in boiling water, removing skin or peeling, decocting, and sun drying.
The product is cylindrical, straight or slightly bent, truncated at two ends, and has a length of 5-18 cm and a diameter of 1-2.5 cm. The surface is white or light brown, bright and clean or has longitudinal wrinkles and fine root marks, and the residual brown crust is occasionally generated. Firm, not easy to break, flat in section, white-like or slightly brownish red, obvious in forming layer ring and radial. Light smell, slightly bitter and sour taste.
The nature and flavor are bitter and sour, and slightly cold. Enter liver and spleen meridians.
Has the functions of nourishing blood, regulating menstruation, astringing yin, stopping sweating, softening liver, relieving pain and suppressing liver yang. Can be used for treating sallow complexion due to blood deficiency, menoxenia, spontaneous perspiration, night sweat, hypochondriac pain, abdominal pain, limb contracture pain, headache and dizziness.
11. Radix Cyathulae:
The product is dry root of Cyathula officinalis Cyathula officinalis Kuan belonging to Amaranthaceae. Collected in autumn and winter, removed from the reed heads, fibrous roots and silt, baked or dried to half dry, piled and moistened, and baked or dried in the sun.
The product is nearly cylindrical, slightly distorted, slightly thinner downwards or with few branches, and has the length of 30-60 cm and the diameter of 0.5-3 cm. The surface is yellow brown or grey brown, and has longitudinal wrinkles, root marks and a plurality of transverse leather hole-like protrusions. Tough, not easy to break, pale yellow or brown in cross section, and the vascular bundles are arranged in a plurality of concentric rings. Light smell, sweet taste.
The nature and flavor are sweet, slightly bitter and flat. It enters liver and kidney meridians.
Has the functions and the main functions of removing blood stasis, dredging channels, promoting the circulation of the joints, promoting urination and treating stranguria. Can be used for treating amenorrhea, abdominal mass, skin disorder, traumatic injury, rheumatalgia, foot flaccidity, tendons contracture, hematuria, and blood stranguria.

Claims (3)

1. A process for identifying main active ingredients of Naomaili granules is characterized by comprising the following steps:
taking 1g of Naomaili granules, grinding, adding 25ml of 70% ethanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, and adding 1ml of absolute ethanol into residues to dissolve the residues to obtain a sample solution;
adding herba Leonuri control 1g into water 50ml, boiling for 30 min, filtering, evaporating filtrate to dryness, adding 70% ethanol 25ml into the residue, and making into medicinal solution;
Taking a stachydrine hydrochloride reference substance, adding absolute ethyl alcohol to prepare a solution containing 1mg per lml as a reference substance solution;
performing thin layer chromatography test;
In the sample chromatogram, the spots with the same color are identified at the positions corresponding to the control chromatogram and the control chromatogram.
2. The process for identifying the main active ingredients of the Naomaili granules according to claim 1, wherein the thin-layer chromatography test comprises the following specific steps:
According to the thin layer chromatography test, 8 μl of the sample solution is sucked, 10 μl of each of the control medicinal material solution and the control solution is respectively spotted on the same silica gel G thin layer plate, acetone-absolute ethyl alcohol-hydrochloric acid is used as developing agent, and the developing agent is developed, taken out, dried in the air, sprayed with the mixed solution of dilute bismuth potassium iodide test solution and ferric trichloride test solution, heated at 105 ℃ for 15 minutes, and inspected under sunlight.
3. The process for identifying the main active ingredients of the Naomaili particles according to claim 2, wherein the process further comprises the steps of preparing a sample solution, respectively precisely sucking 1 μl of a reference substance solution and 1 μl of the sample solution, injecting the sample solution into a liquid chromatograph for measurement to obtain 9 characteristic peaks in the sample chromatograph, corresponding to the retention time of the 9 characteristic peaks in a reference substance chromatograph of a reference medicinal material, calculating the relative retention time of each characteristic peak and the S peak, wherein the peak corresponding to the reference substance peak of leonurine hydrochloride is the S peak, and the relative retention time is within +8% of a specified value.
CN202310760464.1A 2023-06-27 2023-06-27 Process for identifying main active ingredients of Naomaili granules Pending CN119198998A (en)

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