CN112858535A - Radix ophiopogonis producing area identification method - Google Patents

Radix ophiopogonis producing area identification method Download PDF

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CN112858535A
CN112858535A CN202110362660.4A CN202110362660A CN112858535A CN 112858535 A CN112858535 A CN 112858535A CN 202110362660 A CN202110362660 A CN 202110362660A CN 112858535 A CN112858535 A CN 112858535A
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plate
movable
pressing plate
movable groove
groove
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付贤树
计晴阁
李潮锋
王建萍
叶子弘
俞晓平
张明洲
张蓬军
厉巧伟
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China Jiliang University
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China Jiliang University
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract

The invention discloses a method for identifying the producing area of radix ophiopogonis, which comprises the following steps: a. putting the wheat and winter flour and an ethanol water solution with the volume concentration of 85% -95% into a treatment box, and heating, refluxing and leaching completely to obtain a filtrate a; b. concentrating the filtrate a until no alcohol exists, adding deionized water, standing and precipitating at the temperature of 2-10 ℃, taking supernatant, and filtering to obtain filtrate b; c. performing macroporous resin column chromatography on the filtrate b, performing gradient elution by using deionized water, 15-25% ethanol aqueous solution by volume concentration, 25-35% ethanol aqueous solution by volume concentration and 35-45% ethanol aqueous solution by volume concentration in sequence, and collecting effluent liquid; d. measuring the content of ophiopogonin D in the ophiopogonin powder by using an HPLC method; e. and D, detecting whether the effluent liquid in the step c contains the borneol glycoside, and comparing the content of the ophiopogonin D detected in the step D with the content of the ophiopogonin D in the same quality of the Zhejiang ophiopogonis.

Description

Radix ophiopogonis producing area identification method
Technical Field
The invention belongs to the technical field of identification of producing areas of radix ophiopogonis, and particularly relates to an identification method of producing areas of radix ophiopogonis.
Background
Radix Ophiopogonis is also called radix Ophiopogonis, and is dried root tuber of Ophiopogon japonica (L.f) Ker-Gawl. of Liliaceae. Radix Ophiopogonis has effects of nourishing yin, promoting fluid production, moistening lung, and clearing heart fire. It is mainly used for treating dry cough due to lung dryness, tuberculosis due to yin deficiency, sore throat, thirst due to body fluid consumption, internal heat, diabetes, vexation, insomnia, constipation due to intestinal dryness, etc. Radix Ophiopogonis can be divided into Zhejiang radix Ophiopogonis and Chuan radix Ophiopogonis according to different producing areas and varieties. Zhe Mai Dong is mainly produced near Hangzhou and Cixi in Zhejiang province, and the harvesting time limit is generally three years, while Chuan Mai Dong is mainly produced in three counties in Sichuan Mianyang areas, and the harvesting time limit is one year. The Zhe Mai Dong is regarded as genuine herb in all generations, and has the best quality, the Chuan Mai Dong is inferior.
Although the distinction between Zhe ophiopogon root and Chuan ophiopogon root is not made in the item of pharmacopeia ophiopogon root 2015, the superiority of Zhe ophiopogon root as genuine medicinal material is not only shown in the description of the herbs in the past generation, but also in the related literature research. The Chinese medicinal materials of the same basic source have different chemical compositions due to different producing areas, different harvesting seasons and different growth years, so that the quality and the curative effect of the Chinese medicinal materials are influenced. The literature reports also show that the Zhe dwarf lilyturf tuber and the Chuan dwarf lilyturf tuber do not have difference in chemical composition and pharmacy, and the literature researches show that the Zhe dwarf lilyturf tuber is obviously superior to the Chuan dwarf lilyturf tuber in the aspect of immunoregulation on the two aspects of macrophage phagocytosis function and gastrointestinal peristalsis promotion through a zebra fish model. Therefore, in 2015, Zhejiang province processing standard distinguishes Zhejiang ophiopogon root from Chuan ophiopogon root, and Zhejiang ophiopogon root is recorded as an independent item under the 'dwarf lilyturf root' condition. However, the artificial planting of Zhejiang ophiopogon root has long growth years, low yield and poor economic benefit, and the economic development of Zhejiang province and the lack of land resources lead to the fact that the cultivation area of Zhejiang ophiopogon root is smaller and smaller, which results in rare source and high price of Zhejiang ophiopogon root.
The radix Ophiopogonis can be combined with other medicinal materials to make into various Chinese medicinal preparations, such as SHENMAI injection, SHENMAI YIN, SHENMAI Capsule, etc., with radix Ophiopogonis as principal drug, and some prescriptions contain radix Ophiopogonis such as cornu Saigae Tataricae granule for clearing lung-heat, QINGYANRUNHOU pill, QINGYANJIEDU oral liquid, QINGHOUTANG mixture, etc. Market research finds that the traditional Chinese medicine preparation prepared from Zhejiang ophiopogon root is relatively few at present due to the factors of rare source, high price and the like of the Zhejiang ophiopogon root. Therefore, whether the Chinese patent medicine is produced by adopting Zhejiang radix ophiopogonis or not needs to be determined, and the quality of the Zhejiang radix ophiopogonis is identified in the finished product preparation by detection, so that the quality of the Zhejiang radix ophiopogonis is similar to that of the traditional Chinese medicine preparation prepared by using Zhejiang radix ophiopogonis.
At present, national, local standards and pharmaceutical research lack methods for identifying the Zhe radix ophiopogonis in finished preparations, and methods for identifying the Zhe radix ophiopogonis medicinal materials which can be researched in documents and patents, such as appearance discrimination, liquid-phase fingerprint spectrum and other chemical experimental methods, are not suitable for identifying radix ophiopogonis powder, and no particularly clear and effective method for distinguishing the Zhe radix ophiopogonis from the Chuan radix ophiopogonis in finished Chinese medicinal preparations exists at present.
Disclosure of Invention
The invention provides a method for identifying the producing area of radix ophiopogonis in order to overcome the defects of the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme: a method for identifying the producing area of radix ophiopogonis comprises the following steps:
a. putting the wheat and winter flour and an ethanol water solution with the volume concentration of 85% -95% into a treatment box, and heating, refluxing and leaching completely to obtain a filtrate a;
b. concentrating the filtrate a until no alcohol exists, adding deionized water, standing and precipitating at the temperature of 2-10 ℃, taking supernatant, and filtering to obtain filtrate b;
c. performing macroporous resin column chromatography on the filtrate b, performing gradient elution by using deionized water, 15-25% ethanol aqueous solution by volume concentration, 25-35% ethanol aqueous solution by volume concentration and 35-45% ethanol aqueous solution by volume concentration in sequence, and collecting effluent liquid;
d. measuring the content of ophiopogonin D in the ophiopogonin powder by using an HPLC method;
e. d, detecting whether the effluent liquid in the step c contains the borneol glycoside, and comparing the content of the ophiopogonin D detected in the step D with the content of the ophiopogonin D in the same quality of the Zhejiang ophiopogonin; if the detected ophiopogon powder contains the borneol glycoside, the detected ophiopogon powder contains the Zhejiang ophiopogon root component, and if the content of ophiopogonin D in the detected ophiopogon powder is higher than that in equal-quality Zhejiang ophiopogon root, the detected ophiopogon powder is mixed with the radix ophiopogonis;
a cover plate is arranged at the top of the treatment box in the step a, a first groove is formed in the inner wall of the treatment box, a heating block is arranged in the first groove, and a return pipe is arranged on the cover plate; the cover plate is also provided with an air cylinder, a piston rod of the air cylinder is provided with a pressing plate matched with the processing box, the pressing plate is provided with a plurality of first through holes, and the side wall of the processing box is provided with a first motor for driving the pressing plate to rotate; a first connecting block is arranged on the side wall of the treatment box, a first movable cavity is arranged on the first connecting block, a plurality of second connecting blocks matched with the pressing plate are arranged in the first movable cavity, and a water outlet is formed in the bottom of the first movable cavity; the cover plate is provided with a water inlet, the top of the water inlet is provided with a first sealing plate, and the side wall of the treatment box is provided with a feed inlet; when the mixed liquid is obtained, the air cylinder drives the pressing plate to move upwards, the pressing plate rises above the feeding hole, the wheat and winter flour is placed into the treatment box from the feeding hole, after the wheat and winter flour is placed, the ethanol water solution enters the treatment box from the water inlet, after the wheat and winter flour and the ethanol water solution are added, the mixed liquid in the treatment box is heated by the heating block, the first motor drives the pressing plate to rotate, the pressing plate stirs the mixed liquid, and the steam enters the return pipe and then is liquefied and dripped into the treatment box; after the heating reflux is completed, the air cylinder pushes the pressing plate to move downwards, the pressing plate pushes the wheat and winter flour in the solution to move downwards, the wheat and winter flour is pressed at the bottom of the treatment box, the second connecting block is matched with the pressing plate, the mixed liquid at the top of the pressing plate enters the first movable cavity, and the solution is discharged from the water discharge port to obtain filtrate a.
The production places of the radix ophiopogonis are identified by detecting the borneol glycoside and the ophiopogonin D, so that the types of the radix ophiopogonis can be effectively distinguished, whether the radix ophiopogonis powder to be detected is a mixed variety or not can be judged, the identification reliability of the radix ophiopogonis is increased, and the identification accuracy of the production places of the radix ophiopogonis is improved; the pressing plate is matched with the air cylinder, so that the radix ophiopogonis powder is pressed at the bottom of the treatment box after the heating reflux in the treatment box is finished, the phenomenon that the radix ophiopogonis powder blocks filter holes when the radix ophiopogonis powder is filtered is avoided, the solution can be smoothly discharged from a water discharge port, and the difficulty in later cleaning is reduced; the pressing plate is driven to rotate by the first motor, so that the pressing plate also plays a role in stirring the solution in the heating and refluxing process, the wheat and winter flour is uniformly contacted with the solution, and the effectiveness of the extracting solution is ensured; the wheat and winter flour is put into the treatment box through the feed inlet, makes the wheat and winter flour be in the clamp plate below at the beginning promptly to promote the wheat and winter flour in the treatment box when the clamp plate descends and move towards the treatment bottom of the case, realize the separation of wheat and winter flour and solution, thereby quick with the solution from the discharge of treatment incasement, promote the differentiation efficiency to the tuber of dwarf lilyturf.
And c, the macroporous resin in the step c is D101 macroporous resin or D1400 macroporous resin, and the volume loading amount of the macroporous resin is 10-20% of the volume of the filtrate b.
And c, sequentially carrying out gradient elution in the step c by using deionized water, 20% ethanol water solution with volume concentration, 30% ethanol water solution with volume concentration and 40% ethanol water solution with volume concentration.
A first movable groove is formed in the bottom of the pressing plate, a first stirring rod is arranged in the first movable groove, a first sliding block is arranged on the side wall of the first stirring rod, and a first sliding groove matched with the first sliding block is formed in the inner wall of the first movable groove; a second movable groove is formed in the pressing plate, a first connecting rod is arranged in the second movable groove, a first through groove is formed in the top of the second movable groove, a water guide groove matched with the first through groove is formed in the first connecting rod, a first through cavity matched with the first connecting rod is formed in the second connecting rod, and a first push plate used for pushing the first connecting rod to move towards the outside of the second movable groove is arranged at the bottom of the pressing plate; after the pressing plate is driven by the air cylinder to move upwards, the pressing plate is positioned above the feeding hole, the first stirring rod extends out of the first movable groove, the pressing plate is driven by the first motor to rotate, the first stirring rod rotates along with the pressing plate to stir the solution in the treatment box, and the solution is heated and refluxed in the treatment box; after solution heating reflux is accomplished, first motor drive clamp plate rotates, first rotation is to on the corresponding position with the second connecting block, cylinder drive clamp plate downstream, the clamp plate downstream is to handling the bottom of the case portion, the head rod removes to second connecting block one side, first push pedal and first puddler press on the wheat winter flour, first puddler enters into first movable groove, first push pedal moves toward the clamp plate direction, the head rod stretches out from second movable groove, the head rod inserts first logical intracavity, the solution at the clamp plate top enters into the diversion inslot from first logical groove, rivers enter into first movable intracavity along the diversion groove, leachate flows from drain outlet, wheat winter flour stays and handles the incasement, obtain solution an alone.
The bottom of the piston rod of the air cylinder is provided with a third connecting block, the bottom of the third connecting block is provided with a fourth connecting block, the pressing plate is provided with a second groove matched with the fourth connecting block, the third connecting block is sleeved with a connecting ring, the inner wall of the second groove is provided with threads matched with the connecting ring, the side wall of the fourth connecting block is provided with a first connecting plate, the second groove is internally provided with a second connecting plate, and the inner wall of the treatment box is provided with a first limiting block matched with the pressing plate; when the cylinder drives the pressing plate to move upwards, the first limiting block protrudes from the treatment inner surface, the pressing plate moves upwards to the bottom of the first limiting block, the pressing plate cannot move upwards after abutting against the bottom of the first limiting block, a cylinder piston rod drives the fourth connecting block to move upwards relative to the pressing plate, the first connecting plate moves to the position above the second connecting plate, and when the first motor drives the pressing plate to rotate, the fourth connecting block rotates at the top of the second groove; after solution heating reflux is accomplished, cylinder drive piston rod moves down, fourth connecting block moves down along with cylinder piston rod, fourth connecting block removes to second recess bottom, first motor drive clamp plate rotates, the second connecting plate rotates to first connecting plate one side, first connecting plate blocks the second connecting plate and continues to rotate, clamp plate stall back head rod is in the assigned position, the cylinder continues drive piston rod and moves down, the clamp plate moves down and promotes to handle the interior wheat winter flour of incasement and remove to handling the bottom of the case, upper solution is discharged from drain outlet, obtain filtrating a.
The top of the connecting ring is provided with a first connecting spring, the third connecting block is provided with a first cavity and a plurality of third movable grooves communicated with the first cavity, the third movable grooves are internally provided with first limiting rods, the first limiting rods are provided with second connecting springs, the inner wall of the connecting ring is provided with a plurality of fourth movable grooves corresponding to the third movable grooves, the fourth movable grooves are internally provided with air bags, the connecting ring is provided with second movable cavities communicated with the fourth movable grooves, the top of each second movable cavity is provided with a third connecting spring, the bottom of each third connecting spring is provided with a second push plate, and the second push plates penetrate out of the second movable cavities; a fifth movable groove communicated with the first cavity is formed in the fourth connecting block, the first connecting plate is arranged in the fifth movable groove, and a fourth connecting spring is arranged on the first connecting plate; when the press plate is connected to the piston rod of the air cylinder, the fourth connecting block is inserted into the second groove, the connecting ring is positioned at the notch position of the second groove, the first limiting rod is embedded into the fourth movable groove at the moment, the connecting ring and the fourth connecting block form rotation stop fit, the press plate is rotated, the connecting ring and the threads form fit, the connecting ring is fixed on the press plate, the connecting ring moves downwards relative to the press plate when the connecting ring is connected to the press plate, the second push plate abuts against the support ring, the support ring pushes the second push plate to move upwards, the second push plate pushes air in the second movable cavity into the air bag, the air bag pushes the first limiting rod to move towards the third movable groove, the air in the third movable groove is extruded when the first limiting rod moves, the air in the third movable groove enters the first cavity, the air in the first cavity enters the fifth movable groove, and the first connecting plate is pushed by air pressure to extend out from the fifth movable groove, and stopping rotating the pressing plate to complete the connection of the pressing plate and the piston rod of the air cylinder.
A first lug is arranged on the second connecting plate, a third groove matched with the first lug is arranged on the first connecting plate, a sixth movable groove is arranged on the first lug, a limiting spring is arranged in the sixth movable groove, a second limiting block is arranged at one end of the limiting spring, and a seventh movable groove matched with the first lug is arranged on the inner wall of the third groove; an eighth movable groove is formed in the inner wall of the treatment box, the second limiting block is arranged in the eighth movable groove, and a fifth connecting spring is arranged on the first limiting block; a ninth movable groove communicated with the eighth movable groove is formed in the side wall of the treatment box, a third connecting plate is hinged to the side wall of the first limiting block, a fourth connecting plate is hinged to one end of the third connecting plate, a push rod is arranged in the ninth movable groove, a third push plate is arranged at the top of the push rod, and a fourth push plate is arranged at the bottom of the push rod; after the cover plate covers the treatment box, the first limiting block is positioned in the eighth movable groove, the air cylinder driving pressure plate descends to the position below the first limiting block, the third pushing plate is pushed downwards, the third pushing plate drives the fourth pushing plate to move downwards, the fourth pushing plate pushes the third connecting plate and the fourth connecting plate to rotate around a connecting point, the third connecting plate and the fourth connecting plate rotate to push the first limiting block to extend out of the eighth movable groove, the air cylinder driving pressure plate moves upwards, the pressure plate rises to the bottom of the first limiting block, the fourth connecting block moves upwards relative to the pressure plate, the first connecting plate moves to the position above the second connecting plate, the first motor drives the pressure plate to rotate, and the first stirring rod stirs the solution; after solution heating reflux treatment accomplished, cylinder drive fourth connecting block down moved, the fourth connecting block removed to second recess bottom, first motor continues the drive clamp plate and rotates, the second connecting plate rotates to first connecting plate one side, first lug is embedded into the third recess, the second stopper enters into the seventh movable groove, first connecting plate and second connecting plate form fixed connection, the head rod is static on the assigned position, the cylinder continues the drive clamp plate and moves down, solution is discharged from drain outlet.
A connecting shaft is arranged in the first movable cavity, the connecting shaft penetrates through the second connecting block, and the second connecting block is of a disc-shaped structure; the inner wall of the first through cavity is rotatably connected with a sealing door; a tenth movable groove is further formed in the inner wall of the first through cavity, a fifth connecting plate is arranged in the tenth movable groove, a sixth connecting spring is arranged on the fifth connecting plate, a second sealing plate and a second lug are arranged on the fifth connecting plate, the second lug is arranged on one side of the second sealing plate, one end of the second first push block is of an arc-shaped structure, and the second sealing plate and the second lug are arranged in the first through cavity in a penetrating mode; after the solution heating reflux is completed, the pressing plate moves downwards to the bottom of the treatment box, the positions of the second connecting blocks of corresponding quantity are adjusted according to the quantity of the radix ophiopogonis powder put into the treatment box, the second connecting blocks of the specified quantity rotate 180 degrees, the sealing door is rotated into the first movable cavity, the first connecting rod extends out of the second movable groove after the first pushing plate moves upwards, the first connecting rod is inserted into the first through cavity and is in contact with the second lug, the first connecting rod pushes the second lug to move in the tenth movable groove, the fifth connecting plate drives the second connecting plate to move in the tenth movable groove, the solution in the treatment box enters the first through cavity through the diversion groove, the water flow pushes the sealing door to rotate and enter the first movable cavity, and the solution in the first movable cavity is discharged from the water discharge port.
A second through cavity is formed in the top of the first movable cavity, a driving roller matched with the second connecting block penetrates through the second through cavity, a sixth push plate is arranged at the top of the driving roller, and a plurality of annular grooves are formed in the driving roller; an equipment cavity is formed in the first connecting block, a second motor is arranged in the equipment cavity, and a first driving wheel matched with the driving roller is arranged on an output shaft of the second motor; an eleventh movable groove communicated with the second through cavity is formed in the side wall of the second through cavity, a second limiting rod matched with the annular groove is arranged in the eleventh movable groove, a second connecting rod is arranged on the second limiting rod, a reset spring is arranged on the second connecting rod, and the second connecting rod extends out of the eleventh movable groove; after the clamp plate moves to handling the bottom half, promote the second connecting rod toward eleventh activity groove one end, the second gag lever post shifts out from the annular, down promote the sixth push pedal according to the position that the clamp plate was located, the sixth push pedal drives the driving roller and descends to appointed position, second motor drive driving roller rotates, the driving roller drives the second connecting block rotation of appointed number, the second connecting block that is in clamp plate one side rotates 180 degrees, the head rod inserts in the first logical intracavity, the solution at handling roof portion enters into the first activity intracavity from the head rod, solution is discharged from the drain.
A twelfth movable groove is formed in the inner wall of the treatment box, a movable ring is arranged in the twelfth movable groove, a first transmission cavity is formed in the side wall of the twelfth movable groove, and a transmission shaft matched with the movable ring is arranged in the first transmission cavity; a thirteenth movable groove is formed in the top of the twelfth movable groove, a third movable cavity is formed in the movable ring, a plurality of fourteenth movable grooves communicated with the third movable cavity are formed in the inner wall of the movable ring, a seventh connecting spring is arranged in each fourteenth movable groove, a second stirring rod is arranged at one end of each seventh connecting spring, a fifth push plate matched with the thirteenth movable groove penetrates through the third movable cavity, and a supporting spring is arranged at the bottom of each fifth push plate; a fifteenth movable groove communicated with the thirteenth movable groove is formed in the inner wall of the treatment box, an eighth connecting spring is arranged on the inner wall of the fifteenth movable groove, a first push block is arranged at one end of the eighth connecting spring, and cambered surfaces are respectively arranged at the top and the bottom of the first push block; when the cover plate covers the treatment box, the first motor and the transmission shaft form transmission fit; when the pressure plate is in a lifting state, the pressure plate pushes the first push block to move towards the fifteenth movable groove, air in the fifteenth movable groove enters the thirteenth movable groove, the fifth push plate is pushed to move downwards by air pressure, the fifth push plate pushes air in the third movable cavity into the fourteenth movable groove, the second stirring rod extends out of the fourteenth movable groove, the first motor drives the pressure plate to rotate and simultaneously drives the transmission shaft to rotate, the transmission shaft drives the movable ring to rotate, and the first stirring rod and the second stirring rod are matched to stir solution; after solution heating reflux is completed, the air cylinder pushes the pressing plate to move downwards, the pressing plate is moved away from one side of the first pushing block, the first pushing block extends out of the fifteenth movable groove, the second stirring rod enters the fourteenth movable groove, the pressing plate normally moves to the bottom of the processing box, and wheat and winter flour is pressed to collect upper-layer solution after the bottom of the processing box.
The invention has the following advantages: the method has the advantages that the production places of the radix ophiopogonis are identified by detecting the borneol glycoside and the ophiopogonin D, the types of the radix ophiopogonis can be effectively distinguished, whether the radix ophiopogonis powder to be detected is a mixed variety or not can be distinguished, the identification reliability of the radix ophiopogonis is improved, and the identification accuracy of the production places of the radix ophiopogonis is improved.
Drawings
FIG. 1 is a schematic view of the structure of a reaction tank of the present invention.
FIG. 2 is a front view of the reaction chamber of the present invention.
Fig. 3 is a cross-sectional view taken along a-a in fig. 2.
Fig. 4 is an enlarged view of a portion a in fig. 3.
Fig. 5 is an enlarged view at Q in fig. 3.
Fig. 6 is a cross-sectional view taken along line B-B of fig. 2.
Fig. 7 is an enlarged view of fig. 6 at B.
Fig. 8 is a cross-sectional view taken along line C-C of fig. 2.
Fig. 9 is an enlarged view of fig. 8 at C.
Fig. 10 is a cross-sectional view taken along line D-D in fig. 2.
Fig. 11 is an enlarged view of fig. 10 at D.
Fig. 12 is a cross-sectional view taken along line E-E of fig. 2.
Fig. 13 is an enlarged view of fig. 12 at E.
FIG. 14 is a right side view of the reaction chamber of the present invention.
Fig. 15 is a cross-sectional view taken along F-F in fig. 14.
Fig. 16 is an enlarged view of fig. 15 at F.
Fig. 17 is an enlarged view at G in fig. 15.
Fig. 18 is an enlarged view of fig. 17 at H.
Fig. 19 is a cross-sectional view taken along L-L of fig. 14.
Fig. 20 is an enlarged view at I in fig. 19.
Fig. 21 is a cross-sectional view taken along H-H in fig. 14.
Fig. 22 is an enlarged view at J in fig. 21.
Fig. 23 is an enlarged view at K in fig. 22.
Fig. 24 is a cross-sectional view taken along line I-I of fig. 14.
Fig. 25 is an enlarged view at L in fig. 24.
Fig. 26 is a cross-sectional view taken along J-J in fig. 14.
Fig. 27 is an enlarged view of fig. 26 at M.
Fig. 28 is a cross-sectional view taken along line K-K of fig. 14.
Fig. 29 is an enlarged view of fig. 28 at N.
Fig. 30 is an enlarged view at O in fig. 28.
Fig. 31 is an enlarged view at P in fig. 30.
Detailed Description
A method for identifying the producing area of radix ophiopogonis comprises the following steps:
a. putting the wheat and winter flour and an ethanol water solution with the volume concentration of 85% -95% into a treatment box (1), and heating, refluxing and leaching completely to obtain a filtrate a;
b. concentrating the filtrate a until no alcohol exists, adding deionized water, standing and precipitating at the temperature of 2-10 ℃, taking supernatant, and filtering to obtain filtrate b;
c. performing macroporous resin column chromatography on the filtrate b, performing gradient elution by using deionized water, 15-25% ethanol aqueous solution by volume concentration, 25-35% ethanol aqueous solution by volume concentration and 35-45% ethanol aqueous solution by volume concentration in sequence, and collecting effluent liquid;
d. measuring the content of ophiopogonin D in the ophiopogonin powder by using an HPLC method;
e. d, detecting whether the effluent liquid in the step c contains the borneol glycoside, and comparing the content of the ophiopogonin D detected in the step D with the content of the ophiopogonin D in the same quality of the Zhejiang ophiopogonin; if the detected ophiopogon powder contains the borneol glycoside, the detected ophiopogon powder contains the Zhejiang ophiopogon root component, and if the content of ophiopogonin D in the detected ophiopogon powder is higher than that in equal-quality Zhejiang ophiopogon root, the detected ophiopogon powder is mixed with the radix ophiopogonis;
the volume dosage of the leaching liquor in the step a is 2-4L/kg calculated by the mass of the dwarf lilyturf tuber, and the volume dosage of the deionized water in the step b is 2-4L/kg calculated by the addition of the dwarf lilyturf tuber; the macroporous resin in the step c is D101 macroporous resin or D1400 macroporous resin, and the volume of the macroporous resin is 10-20% of the volume of the filtrate b; and c, sequentially carrying out gradient elution in the step c by using deionized water, 20% ethanol water solution with volume concentration, 30% ethanol water solution with volume concentration and 40% ethanol water solution with volume concentration.
As shown in fig. 1-31, a cover plate 2 is arranged on the top of the treatment box 1 in the step a, a first groove is arranged on the inner wall of the treatment box 1, a heating block 18 is arranged in the first groove, and a return pipe 21 is arranged on the cover plate 2; the cover plate 2 is also provided with an air cylinder 26, a piston rod of the air cylinder 26 is provided with a pressing plate 3 matched with the processing box 1, the pressing plate 3 is provided with a plurality of first through holes, and the side wall of the processing box 1 is provided with a first motor for driving the pressing plate 3 to rotate; a first connecting block 11 is arranged on the side wall of the treatment box 1, a first movable cavity is arranged on the first connecting block 11, a plurality of second connecting blocks 19 matched with the pressing plate 3 are arranged in the first movable cavity, and a water outlet is formed in the bottom of the first movable cavity; a water inlet is formed in the cover plate 2, a first sealing plate 27 is arranged at the top of the water inlet, a feed port is formed in the side wall of the treatment box 1, and a third sealing plate is arranged at the feed port; when the mixed liquid is obtained, the air cylinder 26 drives the pressing plate 3 to move upwards, the pressing plate 3 rises above the feeding hole, the wheat and winter flour is placed into the treatment box 1 from the feeding hole, after the wheat and winter flour is placed, the ethanol water solution enters the treatment box 1 from the water inlet, after the wheat and winter flour and the ethanol water solution are added, the mixed liquid in the treatment box 1 is heated by the heating block 18, the first motor drives the pressing plate 3 to rotate, the pressing plate 3 stirs the mixed liquid, and the steam is liquefied and dripped into the treatment box 1 after entering the return pipe 21; after the heating reflux is completed, the air cylinder 26 pushes the pressing plate 3 to move downwards, the pressing plate 3 pushes the wheat and winter flour in the solution to move downwards, the wheat and winter flour is pressed at the bottom of the treatment box 1, the second connecting block 19 is matched with the pressing plate 3, the mixed liquid at the top of the pressing plate 3 enters the first movable cavity, the solution is discharged from the water discharge port, and the filtrate a is obtained.
The pressing plate is matched with the air cylinder, so that the radix ophiopogonis powder is pressed at the bottom of the treatment box after the heating reflux in the treatment box is finished, the phenomenon that the radix ophiopogonis powder blocks filter holes when the radix ophiopogonis powder is filtered is avoided, the solution can be smoothly discharged from a water discharge port, and the difficulty in later cleaning is reduced; the pressing plate is driven to rotate by the first motor, so that the pressing plate also plays a role in stirring the solution in the heating and refluxing process, the wheat and winter flour is uniformly contacted with the solution, and the effectiveness of the extracting solution is ensured; the wheat and winter flour is put into the treatment box through the feed inlet, makes the wheat and winter flour be in the clamp plate below at the beginning promptly to promote the wheat and winter flour in the treatment box when the clamp plate descends and move towards the treatment bottom of the case, realize the separation of wheat and winter flour and solution, thereby quick with the solution from the discharge of treatment incasement, promote the differentiation efficiency to the tuber of dwarf lilyturf.
A first movable groove is formed in the bottom of the pressing plate 3, a first stirring rod 31 is arranged in the first movable groove, a first sliding block is arranged on the side wall of the first stirring rod 31, and a first sliding groove matched with the first sliding block is formed in the inner wall of the first movable groove; under the arrangement of the first sliding block and the first sliding groove, the first stirring rod is prevented from falling out of the first movable groove, and the first stirring rod automatically enters the first movable groove after the pressing plate moves to the bottom of the treatment box; a second movable groove is formed in the pressing plate 3, a first connecting rod 33 is arranged in the second movable groove, a first through groove is formed in the top of the second movable groove, a water guide groove matched with the first through groove is formed in the first connecting rod 33, a first through cavity matched with the first connecting rod 33 is formed in the second connecting block 19, and a first pushing plate 32 used for pushing the first connecting rod 33 to move out of the second movable groove is arranged at the bottom of the pressing plate 3; after the air cylinder 26 drives the pressing plate 3 to move upwards, the pressing plate 3 is positioned above the feeding hole, the first stirring rod 31 extends out of the first movable groove, the first motor drives the pressing plate 3 to rotate, the first stirring rod 31 rotates along with the pressing plate 3 to stir the solution in the treatment box 1, and the solution is heated and refluxed in the treatment box 1; after the solution is heated and reflowed, the first motor drives the pressing plate 3 to rotate, the first rotation is carried out to the position corresponding to the second connecting block 19, the air cylinder 26 drives the pressing plate 3 to move downwards, the pressing plate 3 moves downwards to the bottom of the treatment box 1, the first connecting rod 33 moves to one side of the second connecting block 19, the first pushing plate 32 and the first stirring rod 31 are pressed on the wheat winter wheat flour, the first stirring rod 31 enters the first movable groove, the first pushing plate 32 moves towards the pressing plate 3, the first connecting rod 33 extends out of the second movable groove, the first connecting rod 33 is inserted into the first through cavity, the solution at the top of the pressing plate 3 enters the water diversion groove from the first through groove, the water flow enters the first movable cavity along the water diversion groove, the leaching solution flows out from the water drainage outlet, the wheat winter wheat flour stays in the treatment box 1, and the solution a is obtained independently.
A sixteenth movable groove is formed in the bottom of the pressing plate, a third connecting rod 321 is arranged on the first pushing plate and penetrates through the sixteenth movable groove, a ninth connecting spring 322 is arranged at the top of the third connecting rod, a seventeenth movable groove communicated with the sixteenth movable groove is formed in the side wall of the second movable groove, a fourth connecting rod 331 is arranged on the side wall of the first connecting rod and penetrates through the seventeenth movable groove, and a tenth connecting spring 332 is arranged at one end of the fourth connecting rod; when the first push plate moves upwards, the third connecting rod moves towards the sixteenth movable groove, the third connecting rod pushes air in the sixteenth movable groove to enter the seventeenth movable groove, the fourth connecting rod is pushed to move by air pressure, and the first connecting rod moves along with the fourth connecting rod, so that the first connecting rod extends out of the second movable groove to be connected and matched with the second connecting block; the diversion groove width is greater than first logical groove width, guarantees to lead to the solution homoenergetic that the inslot got into from first leading to in the groove and enters into the diversion groove.
The bottom of the piston rod of the air cylinder 26 is provided with a third connecting block 261, the bottom of the third connecting block 261 is provided with a fourth connecting block 263, the pressing plate 3 is provided with a second groove matched with the fourth connecting block 263, the third connecting block 261 is sleeved with a connecting ring 264, the inner wall of the second groove is provided with threads matched with the connecting ring 264, the side wall of the fourth connecting block 263 is provided with a first connecting plate 2631, the second groove is internally provided with a second connecting plate 35, and the inner wall of the treatment box 1 is provided with a first limiting block 16 matched with the pressing plate 3; when the cylinder 26 drives the pressing plate 3 to move upwards, the first limiting block 16 protrudes from the inner surface to be processed, the pressing plate 3 moves upwards to the bottom of the first limiting block 16, the pressing plate 3 cannot move upwards after abutting against the bottom of the first limiting block 16, the piston rod of the cylinder 26 drives the fourth connecting block 263 to move upwards relative to the pressing plate 3, the first connecting plate 2631 moves to the upper part of the second connecting plate 35, and when the first motor drives the pressing plate 3 to rotate, the fourth connecting block 263 rotates at the top of the second groove; after solution heating reflux is completed, the cylinder 26 drives the piston rod to move downwards, the fourth connecting block 263 moves downwards along with the piston rod of the cylinder 26, the fourth connecting block 263 moves to the bottom of the second groove, the first motor drives the pressing plate 3 to rotate, the second connecting plate 35 rotates to one side of the first connecting plate 2631, the first connecting plate 2631 blocks the second connecting plate 35 to continue rotating, the first connecting rod 33 is located at the designated position after the pressing plate 3 stops rotating, the cylinder 26 continues to drive the piston rod to move downwards, the pressing plate 3 moves downwards to push the wheat and winter flour in the treatment box 1 to move to the bottom of the treatment box 1, the upper-layer solution is discharged from the water outlet, and filtrate a is obtained.
A first connecting spring 262 is arranged at the top of the connecting ring 264, a first cavity and a plurality of third movable grooves communicated with the first cavity are arranged on the third connecting block 261, a first limiting rod 2611 is arranged in the third movable groove, a second connecting spring is arranged on the first limiting rod 2611, a plurality of fourth movable grooves corresponding to the third movable grooves are arranged on the inner wall of the connecting ring 264, an air bag 266 is arranged in the fourth movable groove, a second movable cavity communicated with the fourth movable groove is arranged on the connecting ring 264, a third connecting spring 2651 is arranged at the top of the second movable cavity, a second push plate 265 is arranged at the bottom of the third connecting spring 2651, and the second push plate 265 penetrates out of the second movable cavity; a fifth movable groove communicated with the first cavity is formed in the fourth connecting block 263, the first connecting plate 2631 is arranged in the fifth movable groove, and a fourth connecting spring 2632 is arranged on the first connecting plate 2631; when the pressure plate 3 is connected to the piston rod of the air cylinder 26, the fourth connecting block 263 is inserted into the second groove, the connecting ring 264 is positioned at the notch position of the second groove, at this time, the first limiting rod 2611 is embedded into the fourth movable groove, the connecting ring 264 and the fourth connecting block 263 form a rotation stop fit, the pressure plate 3 is rotated, the connecting ring 264 forms a fit with the thread, the connecting ring 264 is fixed on the pressure plate 3, the connecting ring 264 moves downward relative to the pressure plate 3 when the connecting ring 264 is connected to the pressure plate 3, the second push plate 265 abuts against the support ring 34, the support ring 34 pushes the second push plate 265 to move upward, the second push plate 265 pushes the air in the second movable cavity into the air bag 266, the air bag 266 pushes the first limiting rod 2611 to move into the third movable groove, the air in the third movable groove is pushed when the first limiting rod 2611 moves, the air in the third movable groove enters the first cavity, and the air in the first cavity enters the fifth movable groove, the first connecting plate 2631 is pushed by air pressure to extend out of the fifth movable groove, the pressing plate 3 stops rotating, and the connection between the pressing plate 3 and the piston rod of the air cylinder 26 is completed; the first connecting plate is located in the fifth movable groove when the pressing plate is installed, and normal installation of the pressing plate is prevented from being influenced by collision of the first connecting plate and the second connecting plate when the pressing plate is installed.
An air outlet is formed in the top of the connecting ring, and a fifth sealing plate 267 is arranged at the air outlet; when the pressing plate is detached, the fifth sealing plate is opened, the airflow in the second movable cavity is discharged from the air outlet, the first limiting rod is embedded into the fourth movable groove again after the air bag is contracted, the first connecting block and the connecting ring form rotation stopping fit, the first connecting plate enters the fifth movable groove, the pressing plate is rotated, the pressing plate is detached from the connecting ring, and therefore the pressing plate and the air cylinder are separated.
A first bump 351 is arranged on the second connecting plate 35, a third groove matched with the first bump 351 is arranged on the first connecting plate 2631, a sixth movable groove is arranged on the first bump 351, a limiting spring 352 is arranged in the sixth movable groove, a second limiting block 353 is arranged at one end of the limiting spring 352, a seventh movable groove matched with the first bump 351 is arranged on the inner wall of the third groove, and the first bump can move up and down along the inner wall of the seventh movable groove; an eighth movable groove is formed in the inner wall of the treatment box 1, the second limiting block 353 is arranged in the eighth movable groove, and a fifth connecting spring 163 is arranged on the first limiting block 16; a ninth movable groove communicated with the eighth movable groove is formed in the side wall of the treatment box 1, a third connecting plate 161 is hinged to the side wall of the first limiting block 16, a fourth connecting plate 162 is hinged to one end of the third connecting plate 161, a push rod 171 is arranged in the ninth movable groove, a third push plate 17 is arranged at the top of the push rod 171, and a fourth push plate 172 is arranged at the bottom of the push rod 171; after the cover plate 2 covers the treatment box 1, the first limiting block 16 is positioned in the eighth movable groove, the air cylinder 26 drives the pressing plate 3 to descend below the first limiting block 16 to push the third pressing plate 17 downwards, the third pressing plate 17 drives the fourth pressing plate 172 to move downwards, the fourth pressing plate 172 drives the third connecting plate 161 and the fourth connecting plate 162 to rotate around a connecting point, the third connecting plate 161 and the fourth connecting plate 162 rotate to push the first limiting block 16 to extend out of the eighth movable groove, the air cylinder 26 drives the pressing plate 3 to move upwards, the pressing plate 3 rises to the bottom of the first limiting block 16, the fourth connecting block 263 moves upwards relative to the pressing plate 3, the first connecting plate 2631 moves to above the second connecting plate 35, the first motor drives the pressing plate 3 to rotate, and the first stirring rod 31 stirs the solution; after the solution heating reflux treatment is completed, the cylinder 26 drives the fourth connecting block 263 to move downwards, the fourth connecting block 263 moves to the bottom of the second groove, the first motor continues to drive the platen 3 to rotate, the second connecting plate 35 rotates to one side of the first connecting plate 2631, the first bump 351 is embedded into the third groove, the second limiting block 353 enters the seventh movable groove, the first connecting plate 2631 and the second connecting plate 35 form a fixed connection, the first connecting rod 33 is static at a designated position, the cylinder 26 continues to drive the platen 3 to move downwards, and the solution is discharged from the water discharge port.
A connecting shaft 111 is arranged in the first movable cavity, the connecting shaft 111 penetrates through the second connecting block 19, and the second connecting block 19 is of a disc-shaped structure; a sealing door 191 is rotatably connected to the inner wall of the first through cavity; a tenth movable groove is further formed in the inner wall of the first through cavity, a fifth connecting plate 192 is arranged in the tenth movable groove, a sixth connecting spring 193 is arranged on the fifth connecting plate 192, a second sealing plate 194 and a second lug 195 are arranged on the fifth connecting plate 192, the second lug 195 is arranged on one side of the second sealing plate 194, one end of the second first push block is of an arc-shaped structure, and the second sealing plate 194 and the second lug 195 are arranged in the first through cavity in a penetrating mode; after the solution is heated and reflowed, the pressing plate 3 moves downwards to the bottom of the treatment box 1, the positions of a corresponding number of second connecting blocks 19 are adjusted according to the amount of radix ophiopogonis powder put into the treatment box 1, a specified number of second connecting blocks 19 rotate 180 degrees, the sealing door 191 is switched into a first movable cavity, the first connecting rod 33 extends out of the second movable groove after the first pushing plate 32 moves upwards, the first connecting rod 33 is inserted into the first through cavity, the first connecting rod 33 is in contact with the second lug 195, the first connecting rod 33 pushes the second lug 195 to move into a tenth movable groove, the fifth connecting plate 192 drives the second connecting plate 35 to move into the tenth movable groove, the solution in the treatment box 1 enters the first through groove through the water guide groove, the water flow pushes the sealing door 191 to rotate and enter the first movable cavity, and the solution in the first movable cavity is discharged from the water discharge port.
A second through cavity is formed in the top of the first movable cavity, a driving roller 110 matched with the second connecting block 19 penetrates through the second through cavity, a sixth push plate 1101 is arranged on the top of the driving roller 110, and a plurality of annular grooves are formed in the driving roller 110; an equipment cavity is formed in the first connecting block 11, a second motor 120 is arranged in the equipment cavity, and a first driving wheel 1201 matched with the driving roller 110 is arranged on an output shaft of the second motor 120; an eleventh movable groove communicated with the second through cavity is formed in the side wall of the second through cavity, a second limiting rod 130 matched with the annular groove is arranged in the eleventh movable groove, a second connecting rod 1301 is arranged on the second limiting rod 130, a reset spring 1302 is arranged on the second connecting rod 1301, and the second connecting rod 1301 extends out of the eleventh movable groove; after the pressing plate 3 moves to the bottom of the treatment box 1, the second connecting rod 1301 is pushed towards one end of the eleventh movable groove, the second limiting rod 130 is moved out of the annular groove, the sixth pushing plate 1101 is pushed downwards according to the position where the pressing plate 3 is located, the sixth pushing plate 1101 drives the driving roller 110 to descend to a specified position, the second motor 120 drives the driving roller 110 to rotate, the driving roller 110 drives the second connecting blocks 19 of a specified number to rotate, the second connecting blocks 19 on one side of the pressing plate 3 rotate 180 degrees, the first connecting rods 33 are inserted into the first through cavities, the solution at the top of the treatment box 1 enters the first movable cavities from the first connecting rods 33, and the solution is discharged from the liquid discharge ports.
A twelfth movable groove is formed in the inner wall of the treatment box 1, a movable ring 15 is arranged in the twelfth movable groove, a first transmission cavity is formed in the side wall of the twelfth movable groove, and a transmission shaft 150 matched with the movable ring 15 is arranged in the first transmission cavity; a thirteenth movable groove is formed in the top of the twelfth movable groove, a third movable cavity is formed in the movable ring 15, a plurality of fourteenth movable grooves communicated with the third movable cavity are formed in the inner wall of the movable ring 15, a seventh connecting spring 154 is arranged in the fourteenth movable groove, a second stirring rod 151 is arranged at one end of the seventh connecting spring 154, a fifth push plate 152 matched with the thirteenth movable groove is arranged in the third movable groove in a penetrating manner, and a supporting spring 153 is arranged at the bottom of the fifth push plate 152; a fifteenth movable groove communicated with the thirteenth movable groove is formed in the inner wall of the treatment box 1, an eighth connecting spring 1401 is arranged on the inner wall of the fifteenth movable groove, a first push block 140 is arranged at one end of the eighth connecting spring 1401, and arc surfaces are respectively arranged at the top and the bottom of the first push block 140; when the cover plate 2 is covered on the processing box 1, the first motor and the transmission shaft 150 form transmission fit; when the pressing plate 3 is in a rising state, the pressing plate 3 pushes the first pushing block 140 to move towards the fifteenth movable groove, air in the fifteenth movable groove enters the thirteenth movable groove, the fifth pushing plate 152 is pushed to move downwards by air pressure, the fifth pushing plate 152 pushes air in the third movable cavity into the fourteenth movable groove, the second stirring rod 151 extends out of the fourteenth movable groove, the first motor drives the pressing plate 3 to rotate and simultaneously drives the transmission shaft 150 to rotate, the transmission shaft 150 drives the movable ring 15 to rotate, and the first stirring rod 31 and the second stirring rod 151 are matched to stir solution; after the solution heating reflux is completed, the air cylinder 26 pushes the pressing plate 3 to move downwards, the pressing plate 3 is moved away from one side of the first pushing block 140, the first pushing block 140 extends out of the fifteenth moving groove, the second stirring rod 151 enters the fourteenth moving groove, the pressing plate 3 normally moves to the bottom of the treatment box 1, and the wheat and winter flour is pressed at the bottom of the treatment box 1 and then is collected for the upper solution alone.
A second transmission cavity is arranged on the side wall of the second through cavity, and a second transmission wheel 160 for transmitting the transmission shaft and the pressing plate is arranged in the second transmission cavity; the movable ring and the pressing plate rotate in different directions under the arrangement of the second transmission wheel; the slope of second puddler sets up, can produce up motion rivers when the activity ring drives the second puddler and rotates in handling the incasement, and the rivers of up motion and first puddler produce the collision, increase the contact effect of rivers and wheat winter flour, make more even and solution contact of wheat winter flour.
The bottom of the treatment box is provided with a material carrying plate 14, the side wall of the treatment box is provided with a material outlet, the top of the material outlet is provided with an eighteenth movable groove, a fourth sealing plate 12 is arranged in the eighteenth movable groove, and the fourth sealing plate is provided with a handle; when the pressing plate pushes the dwarf lilyturf tuber powder to move downwards, the dwarf lilyturf tuber powder is pressed on the material carrying plate, after the solution is discharged from the liquid discharge port, the fourth sealing plate is opened, the pressing plate moves upwards for a small distance, and the material carrying plate is taken out from the material discharge port so as to process the dwarf lilyturf tuber powder; after the material carrying plate is taken out, a brush tool can be stretched into the material carrying plate from the discharge port to clean the wheat and winter flour adhered to the bottom surface of the pressing plate.
The reflux pipe is sleeved with a sleeve 22, a second cavity is formed in the side wall of the sleeve, a first partition plate 221 is arranged in the second cavity, and a notch is formed in the top of the first partition plate to enable the two sides of the second cavity to be communicated; a water storage tank 25 is arranged on the cover plate, a second partition plate 255 is arranged in the water storage tank, the second partition plate divides the water storage tank into an upper cavity and a lower cavity, a first water delivery pipe 256 communicated with the second cavity is arranged on the side wall of the lower cavity, and a second water delivery pipe 257 communicated with the second cavity is arranged on the side wall of the upper cavity; a sealing film 251 is arranged on the inner wall of the lower cavity and is made of rubber; a second push block 252 is further arranged in the lower cavity, a third bump 2521 is arranged on the second push block, a second through groove is formed in the second partition plate, a connecting frame 254 is arranged in the upper cavity, a baffle 253 is arranged on the connecting frame, a nineteenth movable groove is formed in the second partition plate, a fifth connecting block 2531 is arranged on the baffle, and a connecting groove matched with the fifth connecting block is formed in the second push block; the first motor is a double-head motor, a third driving wheel 23 is arranged on the other output shaft of the first motor, a fourth driving wheel 24 matched with the third driving wheel is arranged on the cover plate, and a fourth bump 241 matched with the third bump is arranged on the fourth driving wheel; when the first motor works, the fourth driving wheel rotates along with the third driving block, the fourth bump is in discontinuous contact with the third bump, the fourth bump pushes the third bump to move forwards, the second pushing block moves towards the lower cavity, the second pushing block drives the baffle to move when moving, the baffle moves to the top of the second through groove, the second pushing block extrudes water flow in the lower cavity, the water flow in the lower cavity enters the second cavity through the first water pipe, the water flow in the second cavity enters the upper cavity through the second water pipe, and when the fourth bump is not in contact with the third bump, the second pushing block moves backwards, the baffle moves away from the top of the second through groove, the water flow in the upper cavity falls from the second through groove, and the water flow flows to the lower cavity again; the water flow in the second cavity is continuously changed along with the rotation of the fourth driving wheel, the gas entering the backflow pipe is cooled by the water flow, the gas is quickly liquefied and then flows back to the treatment box, the height of the backflow pipe is reduced, and the volume of the treatment box is reduced.
The top of the treatment box is provided with a positioning block 13, the cover plate is provided with a positioning groove matched with the positioning block, and the first motor and the transmission shaft form transmission fit when the cover plate covers the treatment box under the mutual fit of the positioning block and the positioning groove.
The drawings in the application are only schematic and the specific dimensions thereof are subject to practical implementation.

Claims (10)

1. The method for identifying the producing area of the radix ophiopogonis is characterized by comprising the following steps: the method comprises the following steps:
a. putting the wheat and winter flour and an ethanol water solution with the volume concentration of 85% -95% into a treatment box (1), and heating, refluxing and leaching completely to obtain a filtrate a;
b. concentrating the filtrate a until no alcohol exists, adding deionized water, standing and precipitating at the temperature of 2-10 ℃, taking supernatant, and filtering to obtain filtrate b;
c. performing macroporous resin column chromatography on the filtrate b, performing gradient elution by using deionized water, 15-25% ethanol aqueous solution by volume concentration, 25-35% ethanol aqueous solution by volume concentration and 35-45% ethanol aqueous solution by volume concentration in sequence, and collecting effluent liquid;
d. measuring the content of ophiopogonin D in the ophiopogonin powder by using an HPLC method;
e. d, detecting whether the effluent liquid in the step c contains the borneol glycoside, and comparing the content of the ophiopogonin D detected in the step D with the content of the ophiopogonin D in the same quality of the Zhejiang ophiopogonin; if the detected ophiopogon powder contains the borneol glycoside, the detected ophiopogon powder contains the Zhejiang ophiopogon root component, and if the content of ophiopogonin D in the detected ophiopogon powder is higher than that in equal-quality Zhejiang ophiopogon root, the detected ophiopogon powder is mixed with the radix ophiopogonis;
a cover plate (2) is arranged at the top of the treatment box (1) in the step a, a first groove is formed in the inner wall of the treatment box (1), a heating block (18) is arranged in the first groove, and a return pipe (21) is arranged on the cover plate (2); the cover plate (2) is further provided with an air cylinder (26), a piston rod of the air cylinder (26) is provided with a pressing plate (3) matched with the processing box (1), the pressing plate (3) is provided with a plurality of first through holes, and the side wall of the processing box (1) is provided with a first motor for driving the pressing plate (3) to rotate; a first connecting block (11) is arranged on the side wall of the treatment box (1), a first movable cavity is arranged on the first connecting block (11), a plurality of second connecting blocks (19) matched with the pressing plate (3) are arranged in the first movable cavity, and a water outlet is formed in the bottom of the first movable cavity; a water inlet is formed in the cover plate (2), a first sealing plate (27) is arranged at the top of the water inlet, and a feeding hole is formed in the side wall of the treatment box (1); when the mixed liquid is obtained, the air cylinder (26) drives the pressing plate (3) to move upwards, the pressing plate (3) rises above the feeding hole, the wheat and winter flour is placed into the treatment box (1) from the feeding hole, after the wheat and winter flour is placed, the ethanol water solution enters the treatment box (1) from the water inlet, after the wheat and winter flour and the ethanol water solution are added, the heating block (18) heats the mixed liquid in the treatment box (1), the first motor drives the pressing plate (3) to rotate, the pressing plate (3) stirs the mixed liquid, and the steam is liquefied and dropped into the treatment box (1) after entering the return pipe (21); after the heating reflux is completed, the air cylinder (26) pushes the pressing plate (3) to move downwards, the pressing plate (3) pushes the wheat and winter flour in the solution to move downwards, the wheat and winter flour is pressed at the bottom of the treatment box (1), the second connecting block (19) and the pressing plate (3) form matching, mixed liquid at the top of the pressing plate (3) enters the first movable cavity, and the solution is discharged from the water drainage port to obtain filtrate a.
2. The method for identifying the producing area of ophiopogon japonicus according to claim 1, wherein: and c, the macroporous resin in the step c is D101 macroporous resin or D1400 macroporous resin, and the volume loading amount of the macroporous resin is 10-20% of the volume of the filtrate b.
3. The method for identifying the producing area of ophiopogon japonicus according to claim 1, wherein: and c, sequentially carrying out gradient elution in the step c by using deionized water, 20% ethanol water solution with volume concentration, 30% ethanol water solution with volume concentration and 40% ethanol water solution with volume concentration.
4. The method for identifying the producing area of ophiopogon japonicus according to claim 1, wherein: a first movable groove is formed in the bottom of the pressing plate (3), a first stirring rod (31) is arranged in the first movable groove, a first sliding block is arranged on the side wall of the first stirring rod (31), and a first sliding groove matched with the first sliding block is formed in the inner wall of the first movable groove; a second movable groove is formed in the pressing plate (3), a first connecting rod (33) is arranged in the second movable groove, a first through groove is formed in the top of the second movable groove, a water guide groove matched with the first through groove is formed in the first connecting rod (33), a first through cavity matched with the first connecting rod (33) is formed in the second connecting block (19), and a first push plate (32) used for pushing the first connecting rod (33) to move towards the outside of the second movable groove is arranged at the bottom of the pressing plate (3); after the cylinder (26) drives the pressing plate (3) to move upwards, the pressing plate (3) is located above the feeding hole, the first stirring rod (31) extends out of the first movable groove, the first motor drives the pressing plate (3) to rotate, the first stirring rod (31) rotates along with the pressing plate (3) to stir the solution in the treatment box (1), and the solution is heated and refluxed in the treatment box (1); after the solution is heated and reflowed, a first motor drives a pressing plate (3) to rotate, the first rotation is carried out to the position corresponding to a second connecting block (19), a cylinder (26) drives the pressing plate (3) to move downwards, the pressing plate (3) moves downwards to the bottom of a treatment box (1), a first connecting rod (33) moves to one side of the second connecting block (19), a first pushing plate (32) and a first stirring rod (31) are pressed on the wheat and winter wheat flour, the first stirring rod (31) enters a first movable groove, the first pushing plate (32) moves towards the direction of the pressing plate (3), the first connecting rod (33) extends out of the second movable groove, the first connecting rod (33) is inserted into a first through cavity, the solution at the top of the pressing plate (3) enters a water diversion groove from the first through groove, water flow enters the first movable cavity along the water diversion groove, leachate flows out from a water outlet, the wheat and winter wheat flour stays in the treatment box (1), solution a was obtained separately.
5. The method for identifying the producing area of ophiopogon japonicus according to claim 1, wherein: a third connecting block (261) is arranged at the bottom of a piston rod of the air cylinder (26), a fourth connecting block (263) is arranged at the bottom of the third connecting block (261), a second groove matched with the fourth connecting block (263) is formed in the pressing plate (3), a connecting ring (264) is sleeved on the third connecting block (261), threads matched with the connecting ring (264) are formed in the inner wall of the second groove, a first connecting plate (2631) is arranged on the side wall of the fourth connecting block (263), a second connecting plate (35) is arranged in the second groove, and a first limiting block (16) matched with the pressing plate (3) is arranged on the inner wall of the treatment box (1); when the cylinder (26) drives the pressing plate (3) to move upwards, the first limiting block (16) protrudes from the treatment inner surface, the pressing plate (3) moves upwards to the bottom of the first limiting block (16), the pressing plate (3) cannot move upwards after abutting against the bottom of the first limiting block (16), a piston rod of the cylinder (26) drives the fourth connecting block (263) to move upwards relative to the pressing plate (3), the first connecting plate (2631) moves to the position above the second connecting plate (35), and when the first motor drives the pressing plate (3) to rotate, the fourth connecting block (263) rotates at the top of the second groove; after solution heating reflux is completed, the cylinder (26) drives the piston rod to move downwards, the fourth connecting block (263) moves downwards along with the piston rod of the cylinder (26), the fourth connecting block (263) moves to the bottom of the second groove, the first motor drives the pressing plate (3) to rotate, the second connecting plate (35) rotates to one side of the first connecting plate (2631), the first connecting plate (2631) blocks the second connecting plate (35) to continue rotating, the first connecting plate (33) is located at a specified position after the pressing plate (3) stops rotating, the cylinder (26) continues to drive the piston rod to move downwards, the pressing plate (3) moves downwards to push wheat and winter flour in the treatment box (1) to move to the bottom of the treatment box (1), and upper-layer solution is discharged from a drainage port to obtain filtrate a.
6. The method for identifying the producing area of ophiopogon japonicus according to claim 5, wherein: the top of the connecting ring (264) is provided with a first connecting spring (262), the third connecting block (261) is provided with a first cavity and a plurality of third movable grooves communicated with the first cavity, the third movable grooves are internally provided with first limiting rods (2611), the first limiting rods (2611) are provided with second connecting springs, the inner wall of the connecting ring (264) is provided with a plurality of fourth movable grooves corresponding to the third movable grooves, the fourth movable grooves are internally provided with air bags (266), the connecting ring (264) is provided with second movable cavities communicated with the fourth movable grooves, the top of the second movable cavities is provided with a third connecting spring (2651), the bottom of the third connecting spring (2651) is provided with a second push plate (265), and the second push plate (265) penetrates out of the second movable cavities; a fifth movable groove communicated with the first cavity is formed in the fourth connecting block (263), the first connecting plate (2631) is arranged in the fifth movable groove, and a fourth connecting spring (2632) is arranged on the first connecting plate (2631); when the pressure plate (3) is connected to the piston rod of the air cylinder (26), the fourth connecting block (263) is inserted into the second groove, the connecting ring (264) is positioned at the notch position of the second groove, the first limiting rod (2611) is embedded into the fourth movable groove at the moment, the connecting ring (264) and the fourth connecting block (263) form rotation stop fit, the pressure plate (3) is rotated, the connecting ring (264) forms fit with the threads, the connecting ring (264) is fixed on the pressure plate (3), the connecting ring (264) moves downwards relative to the pressure plate (3) when the connecting ring (264) is connected to the pressure plate (3), the second push plate (265) abuts against the support ring (34), the support ring (34) pushes the second push plate (265) to move upwards, the second push plate (265) pushes air in the second movable cavity into the air bag (266), and the air bag (266) pushes the first limiting rod (2611) to move inwards the third movable groove, when the first limiting rod (2611) moves, air in the third movable groove is extruded, the air in the third movable groove enters the first cavity, the air in the first cavity enters the fifth movable groove, the first connecting plate (2631) is pushed by air pressure to stretch out of the fifth movable groove, the pressing plate (3) stops rotating, and the connection of the pressing plate (3) and the piston rod of the air cylinder (26) is completed.
7. The method for identifying the producing area of ophiopogon japonicus according to claim 6, wherein: a first bump (351) is arranged on the second connecting plate (35), a third groove matched with the first bump (351) is arranged on the first connecting plate (2631), a sixth movable groove is arranged on the first bump (351), a limiting spring (352) is arranged in the sixth movable groove, a second limiting block (353) is arranged at one end of the limiting spring (352), and a seventh movable groove matched with the first bump (351) is arranged on the inner wall of the third groove; an eighth movable groove is formed in the inner wall of the treatment box (1), the second limiting block (353) is arranged in the eighth movable groove, and a fifth connecting spring (163) is arranged on the first limiting block (16); a ninth movable groove communicated with the eighth movable groove is formed in the side wall of the treatment box (1), a third connecting plate (161) is hinged to the side wall of the first limiting block (16), a fourth connecting plate (162) is hinged to one end of the third connecting plate (161), a push rod (171) is arranged in the ninth movable groove, a third push plate (17) is arranged at the top of the push rod (171), and a fourth push plate (172) is arranged at the bottom of the push rod; after the cover plate (2) covers the treatment box (1), the first limiting block (16) is positioned in an eighth movable groove, the cylinder (26) drives the pressing plate (3) to fall below the first limiting block (16) to push a third pushing plate (17) downwards, the third pushing plate (17) drives a fourth pushing plate (172) to move downwards, the fourth pushing plate (172) pushes a third connecting plate (161) and a fourth connecting plate (162) to rotate around a connecting point, the third connecting plate (161) and the fourth connecting plate (162) rotate to push the first limiting block (16) to extend out of the eighth movable groove, the cylinder (26) drives the pressing plate (3) to move upwards, the pressing plate (3) rises to the bottom of the first limiting block (16), the fourth connecting block (263) moves upwards relative to the pressing plate (3), the first connecting plate (2631) moves to the upper side of the second connecting plate (35), and the first motor drives the pressing plate (3) to rotate, the first stirring rod (31) stirs the solution; after the solution heating reflux treatment is completed, the cylinder (26) drives the fourth connecting block (263) to move downwards, the fourth connecting block (263) moves to the bottom of the second groove, the first motor continues to drive the pressing plate (3) to rotate, the second connecting plate (35) rotates to one side of the first connecting plate (2631), the first bump (351) is embedded into the third groove, the second limiting block (353) enters the seventh movable groove, the first connecting plate (2631) and the second connecting plate (35) form a fixed connection, the first connecting rod (33) is static at a specified position, the cylinder (26) continues to drive the pressing plate (3) to move downwards, and the solution is discharged from the water discharge port.
8. The method for identifying the producing area of ophiopogon japonicus according to claim 1, wherein: a connecting shaft (111) is arranged in the first movable cavity, the connecting shaft (111) penetrates through the second connecting block (19), and the second connecting block (19) is of a disc-shaped structure; a sealing door (191) is rotatably connected to the inner wall of the first through cavity; a tenth movable groove is further formed in the inner wall of the first through cavity, a fifth connecting plate (192) is arranged in the tenth movable groove, a sixth connecting spring (193) is arranged on the fifth connecting plate (192), a second sealing plate (194) and a second bump (195) are arranged on the fifth connecting plate (192), the second bump (195) is arranged on one side of the second sealing plate (194), one end of the second first push block is of an arc-shaped structure, and the second sealing plate (194) and the second bump (195) are arranged in the first through cavity in a penetrating mode; after the solution is heated and reflowed, the pressing plate (3) moves downwards to the bottom of the treatment box (1), the positions of a corresponding number of second connecting blocks (19) are adjusted according to the amount of radix ophiopogonis powder put into the treatment box (1), a specified number of second connecting blocks (19) rotate 180 degrees, the sealing door (191) is shifted into a first movable cavity, after the first pushing plate (32) moves upwards, the first connecting rod (33) extends out of the second movable groove, the first connecting rod (33) is inserted into the first through cavity, the first connecting rod (33) is in contact with the second lug (195), the first connecting rod (33) pushes the second lug (195) to move into the tenth movable groove, the fifth connecting plate (192) drives the second connecting plate (35) to move into the tenth movable groove, the solution in the treatment box (1) enters the first through groove through the water guide groove, and the water flow pushes the sealing door (191) to rotate into the first movable cavity, the solution in the first movable cavity is discharged from the water outlet.
9. The method for identifying the producing area of ophiopogon root according to claim 8, wherein: a second through cavity is formed in the top of the first movable cavity, a driving roller (110) matched with the second connecting block (19) penetrates through the second through cavity, a sixth push plate (1101) is arranged on the top of the driving roller (110), and a plurality of annular grooves are formed in the driving roller (110); an equipment cavity is formed in the first connecting block (11), a second motor (120) is arranged in the equipment cavity, and a first driving wheel (1201) matched with the driving roller (110) is arranged on an output shaft of the second motor (120); an eleventh movable groove communicated with the second through cavity is formed in the side wall of the second through cavity, a second limiting rod (130) matched with the annular groove is arranged in the eleventh movable groove, a second connecting rod (1301) is arranged on the second limiting rod (130), a return spring (1302) is arranged on the second connecting rod (1301), and the second connecting rod (1301) extends out of the eleventh movable groove; after the pressing plate (3) moves to the bottom of the treatment box (1), a second connecting rod (1301) is pushed to one end of an eleventh movable groove, a second limiting rod (130) is moved out of the annular groove, a sixth pushing plate (1101) is pushed downwards according to the position where the pressing plate (3) is located, the sixth pushing plate (1101) drives the driving roller (110) to descend to a specified position, the second motor (120) drives the driving roller (110) to rotate, the driving roller (110) drives a specified number of second connecting blocks (19) to rotate, the second connecting blocks (19) on one side of the pressing plate (3) rotate 180 degrees, the first connecting rods (33) are inserted into the first through cavities, the solution on the top of the treatment box (1) enters the first movable cavities from the first connecting rods (33), and the solution is discharged from the liquid discharge ports.
10. The method for identifying the producing area of ophiopogon japonicus according to claim 1, wherein: a twelfth movable groove is formed in the inner wall of the treatment box (1), a movable ring (15) is arranged in the twelfth movable groove, a first transmission cavity is formed in the side wall of the twelfth movable groove, and a transmission shaft (150) matched with the movable ring (15) is arranged in the first transmission cavity; a thirteenth movable groove is formed in the top of the twelfth movable groove, a third movable cavity is formed in the movable ring (15), a plurality of fourteenth movable grooves communicated with the third movable cavity are formed in the inner wall of the movable ring (15), a seventh connecting spring (154) is arranged in the fourteenth movable groove, a second stirring rod (151) is arranged at one end of the seventh connecting spring (154), a fifth push plate (152) matched with the thirteenth movable groove penetrates through the third movable cavity, and a supporting spring (153) is arranged at the bottom of the fifth push plate (152); a fifteenth movable groove communicated with the thirteenth movable groove is formed in the inner wall of the treatment box (1), an eighth connecting spring (1401) is arranged on the inner wall of the fifteenth movable groove, a first push block (140) is arranged at one end of the eighth connecting spring (1401), and arc surfaces are respectively arranged at the top and the bottom of the first push block (140); when the cover plate (2) covers the treatment box (1), the first motor and the transmission shaft (150) form transmission fit; when the pressure plate (3) is in a lifting state, the pressure plate (3) pushes the first push block (140) to move towards the fifteenth movable groove, air in the fifteenth movable groove enters the thirteenth movable groove, the fifth push plate (152) is pushed to move downwards by air pressure, the fifth push plate (152) pushes air in the third movable cavity into the fourteenth movable groove, the second stirring rod (151) extends out of the fourteenth movable groove, the first motor drives the pressure plate (3) to rotate and simultaneously drives the transmission shaft (150) to rotate, the transmission shaft (150) drives the movable ring (15) to rotate, and the first stirring rod (31) and the second stirring rod (151) are matched to stir solution; after solution heating reflux is completed, the air cylinder (26) pushes the pressing plate (3) to move downwards, the pressing plate (3) is moved away from one side of the first pushing block (140), the first pushing block (140) extends out of the fifteenth movable groove, the second stirring rod (151) enters the fourteenth movable groove, the pressing plate (3) normally moves to the bottom of the treatment box (1), and wheat and winter flour is pressed to collect the upper-layer solution independently after the bottom of the treatment box (1).
CN202110362660.4A 2021-04-02 2021-04-02 Radix ophiopogonis producing area identification method Withdrawn CN112858535A (en)

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CN102243170A (en) * 2010-05-12 2011-11-16 天津天士力现代中药资源有限公司 Method for identifying production place of dwarf lilyturf root by using near infrared spectrum technology
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CN103540674B (en) * 2013-10-30 2015-07-22 中国中医科学院中药研究所 Method for authenticating geo-authentic crude drug radix ophiopogonis in different producing areas and kit for method
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113358599A (en) * 2021-06-07 2021-09-07 浙江育英职业技术学院 West lake Longjing traceability technology based on new retail mode

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Application publication date: 20210528