CN112915584B - Extraction method and extraction device for heavy metal detection pretreatment in Tibetan medicinal materials - Google Patents

Extraction method and extraction device for heavy metal detection pretreatment in Tibetan medicinal materials Download PDF

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CN112915584B
CN112915584B CN202110089746.4A CN202110089746A CN112915584B CN 112915584 B CN112915584 B CN 112915584B CN 202110089746 A CN202110089746 A CN 202110089746A CN 112915584 B CN112915584 B CN 112915584B
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extraction
reagent
pipeline
pipe
tibetan
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CN112915584A (en
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王福清
张丽云
许波
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Tibet Tianhong Technology Co ltd
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Tibet Tianhong Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/04Solvent extraction of solutions which are liquid
    • B01D11/0492Applications, solvents used
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/04Solvent extraction of solutions which are liquid
    • B01D11/0476Moving receptacles, e.g. rotating receptacles
    • B01D11/048Mixing by counter-current streams provoked by centrifugal force, in rotating coils or in other rotating spaces

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Abstract

The invention discloses an extraction method and an extraction device for detection pretreatment of heavy metals in Tibetan medicines, wherein the extraction device comprises: the support, the reagent tank group, the pipeline conveying device, the over-current prevention device and the extraction pipe group are sequentially arranged in the reagent flowing direction; the pipeline conveying device comprises a plurality of first pipelines and second pipelines, and the first pipelines and the second pipelines form a plurality of independent flowing spaces and discharge ends of reagents; the over-current prevention device comprises a shell, a plurality of support plates, a plurality of adjusting structures and a blocking structure; the support plate is provided with a first sliding groove and a limiting groove; the adjusting structure comprises a plurality of coaxially sleeved sliding rods, each sliding rod is provided with a limiting rod, each sliding rod is provided with a second sliding groove for the limiting rod of the corresponding sliding rod to slide, and the limiting rods are clamped in limiting grooves with different heights from top to bottom; the blocking structure comprises a plurality of sealing plates for blocking a plurality of reagent discharging ends. The extraction device is used for extracting the digestion solution of the Tibetan medicine materials, the pollution in the extraction process is small, parallel samples can be simultaneously manufactured, and the test efficiency is high.

Description

Extraction method and extraction device for heavy metal detection pretreatment in Tibetan medicinal materials
Technical Field
The invention relates to the technical field of heavy metal detection pretreatment in Tibetan medicinal materials. More particularly, the invention relates to an extraction method and an extraction device for detection pretreatment of heavy metals in Tibetan medicinal materials.
Background
The Tibetan medicinal materials are traditional Chinese medicinal materials in Tibetan regions, are various in types, comprise cordyceps sinensis, snow lotus herb, rhodiola rosea, saffron and the like, and have great research significance. Heavy metal pollution in the Tibetan medicine is an important reason for reducing the quality of the Tibetan medicine, and when the Tibetan medicine is used as the medicine, the influence of toxic heavy metal in the Tibetan medicine on human health is concerned by more and more scholars. Therefore, the current situation of the sources of heavy metals in the Tibetan medicinal materials is analyzed, scientific research on the Tibetan medicinal materials is enhanced, the toxicity of the Tibetan medicinal materials is reduced, scientific and reasonable limit standards and detection methods are provided, and the method has positive significance for promoting the modernization and internationalization of Chinese herbal medicines. At present, before the Tibetan medicines are subjected to heavy metal detection, the Tibetan medicines are digested by strong acid or directly extracted or extracted after digestion, and then extracted, and the subsequent heavy metal detection is carried out without a hydrolysate or an extract liquid, for example, in the text of the detection method of heavy metals in Chinese herbal medicines, the Chinese herbal medicines are firstly digested by strong acid, then extracted by Schiff base, fatty alcohol-polyoxyethylene ether and the like, and the heavy metals are enriched for subsequent detection; in the pretreatment of heavy metal detection in the Tibetan medicinal materials, instruments such as a separating funnel, a graduated test tube and a centrifuge tube are usually adopted for extraction operation, then centrifugal layering or static layering is carried out, and target extract is taken for heavy metal detection. Due to different types of added reagents, the reagents need to be added for multiple times and transferred for multiple times, the problems of pollution or reagent volatilization and the like can be caused in the reagent transferring process, parallel samples cannot be simultaneously manufactured, and the test operation is complicated and long in time.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and to provide an extraction apparatus for pretreatment of heavy metal detection in Tibetan medicines, which is low in pollution during extraction, can simultaneously produce parallel samples, and is high in test efficiency.
To achieve these objects and other advantages and in accordance with the purpose of the invention, there is provided an extraction device for heavy metal detection pretreatment in Tibetan medicine for extracting a Tibetan medicine digestion solution, comprising:
the support comprises a lower support and an upper support which are connected in a telescopic manner;
the reagent tank group is arranged on the upper bracket and comprises a plurality of reagent tanks which are vertically arranged side by side, and a discharge hole is formed in the bottom of each reagent tank; the extraction pipe group is arranged on the lower support and comprises a plurality of extraction pipes which are vertically arranged side by side, adjacent extraction pipes are fixedly connected through a connecting shaft, and the extraction pipe group drives the connecting shaft to operate through a motor; scales are arranged on the outer wall of the extraction tube;
a fluid guide group which is arranged between the reagent tank group and the extraction tube group and communicates the reagent tank group and the extraction tube group; the fluid diversion set comprises a pipeline conveying device and an overflow prevention device; the pipeline conveying device is arranged below the reagent tank group and comprises a plurality of first pipelines and second pipelines, one first pipeline is communicated with one reagent tank through the discharge port to flow one reagent, the second pipeline comprises a horizontal main pipeline and a plurality of vertical branch pipelines which are integrally formed, the main pipeline and the branch pipelines respectively comprise a plurality of pipe bodies which are coaxially sleeved to form independent annular flowing spaces of the plurality of reagents, the plurality of annular flowing spaces of the main pipeline are respectively communicated with the plurality of first pipelines, and the lower end of each branch pipeline forms the discharge end of the plurality of reagents; the lower end of each branch pipeline is communicated with an extraction pipe through an overflow prevention device; the over-flow prevention device is arranged above the extraction tube and comprises a shell, a plurality of support plates, a plurality of adjusting structures and a blocking structure; the top of the shell is detachably connected with the branch pipeline, an adjusting structure is arranged on the shell through a support plate, and the support plate is provided with a vertical first chute and a transverse limiting groove communicated with the first chute; the adjusting structure comprises a plurality of coaxially sleeved slide bars vertically penetrating through the shell, a limiting rod is arranged on the outer side of each slide bar, a second sliding groove for the limiting rod of one slide bar in the slide bar to slide up and down is formed in each slide bar, and the limiting rods sleeved with the slide bars from outside to inside are clamped in the transverse limiting grooves at different heights from top to bottom; the blocking structure comprises a plurality of sealing plates for blocking the discharge ends of a plurality of reagents of the branch pipelines, the sealing plate at the lowest part is of a circular structure, the sealing plate above the circular structure is of an annular structure with sequentially increasing outer diameters from bottom to top, and one side of each sealing plate is fixedly connected with the bottom of one sliding rod;
the interval of horizontal spacing groove sets up to: when the height of a limiting rod is increased to enable the sealing plate to be located at the preset height, the discharge end of a reagent of the branch pipeline is sealed.
Preferably, a horizontal support plate is fixedly connected to the top of each support plate, and the horizontal support plate faces the sliding rod; each limit rod is fixedly connected with the horizontal support plate through a spring; when the limiting rod is clamped in the transverse limiting groove, the spring is in a stretching state.
Preferably, the device also comprises a discharging mechanism, wherein the discharging mechanism comprises a discharging pipe detachably connected with the bottom of the extraction pipe, a material guide pipe penetrating through the outer wall of the discharging pipe, and a buffer tank fixedly connected with the free end part of the material guide pipe; a liquid outlet is formed in the bottom of the buffer tank, and a valve is arranged at the liquid outlet; the inside of the discharging pipe is provided with a piston plate which is connected with the inner wall of the discharging pipe in a sealing and sliding manner, the height of the piston plate is the same as the diameter of the liquid outlet, one surface of the piston plate, which is far away from the extraction pipe, is provided with a piston rod, and the piston plate moves up and down along the discharging pipe to control the discharging flow rate of the discharging pipe.
Preferably, the cross section of the discharge pipe is square.
Preferably, a lifting handle shaped like a letter 21274is arranged above the reagent pot group, and two ends of the lifting handle shaped like the letter 21274are fixedly connected with the upper bracket.
Preferably, the outer surface of the sealing plate is coated with a sealing layer.
An extraction method for detection pretreatment of heavy metals in Tibetan medicinal materials is characterized in that an extraction device for detection pretreatment of heavy metals in Tibetan medicinal materials is adopted to extract digestion solution of Tibetan medicinal materials, and the extraction method comprises the following specific steps:
s1, adding a reagent into the reagent tank;
s2, adding the reagent in the S1 into the extraction tube through the fluid diversion group;
and S3, starting the motor, rotating the extraction tube in the S2, extracting for 5-10min, and collecting the target extraction liquid.
The invention at least comprises the following beneficial effects:
1. according to the invention, by designing the reagent tank group and the pipeline conveying device, an independent circulation space is provided for each reagent raw material, and the problems of pollution, volatilization and the like generated in the transfer process of the reagent are avoided; by designing the over-current prevention device, under the condition that the time for reagents to enter different extraction tubes is inconsistent, the discharge end where the reagent which preferentially reaches the target volume is located can be closed by using the blocking structure, so that test errors caused by different feeding amounts due to the inconsistent time for the reagents to enter the extraction tubes at different discharge ends are avoided; by designing the motor and the extraction pipe group, a plurality of parallel samples can be prepared simultaneously, and the extraction efficiency is improved; the invention can improve the test efficiency and test accuracy of the subsequent detection of the heavy metals of the Tibetan medicinal materials by extracting the heavy metals of the Tibetan medicinal material digestion solution.
2. By designing the piston plate, the piston rod, the material guide pipe, the liquid outlet and the valve, the discharging speed of the target extraction liquid can be effectively controlled when the target extraction liquid is collected; through designing the buffer tank, the target extraction liquid that can let the outflow buffers through the buffer tank, avoids the extraction liquid velocity of flow too fast to cause the separation effect poor, improves follow-up heavy metal detection test's accuracy nature.
3. According to the invention, by designing the horizontal support plate and the spring, when the limiting rod is moved to the first sliding groove, the sealing plate at the bottom of the sliding rod can be driven to move upwards under the action of the spring, so that the operation is convenient, and the efficiency is high.
4. According to the invention, the 21274; shaped handle is designed on the upper bracket, so that the upper bracket can be conveniently taken, and the practicability of the device is improved.
5. According to the invention, the sealing layer is coated on the outer surface of the sealing plate, so that test errors caused by the fact that redundant reagents flow into the extraction tube are effectively prevented.
6. The invention provides an extraction method for detection pretreatment of heavy metals in Tibetan medicinal materials, which is characterized in that an extraction device for detection pretreatment of heavy metals in Tibetan medicinal materials is used for extracting digestion liquid of the Tibetan medicinal materials, so that the pollution in the extraction process is small, parallel samples can be simultaneously manufactured, and the test efficiency is high.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1 is a schematic structural diagram of an extraction device for heavy metal detection pretreatment in Tibetan medicines according to one technical scheme of the present invention;
FIG. 2 is an enlarged view of FIG. 1 at A;
FIG. 3 is an enlarged view of FIG. 1 at B;
FIG. 4 is an enlarged view of FIG. 1 at C;
FIG. 5 is a cross-sectional view of the discharge end of one embodiment of the present invention;
fig. 6 is a top view of an overcurrent prevention device according to one embodiment of the present invention;
d, E, F in FIG. 7 are side views of the first, second and third slide bars, respectively, according to one of the technical solutions of the present invention;
FIG. 8 is a side view of one embodiment of the plate of the present invention.
Reference numerals: 1-lower support; 2-an extraction tube; 3-reagent tank; 4-a first valve; 5-a first circulation conduit; 6-a second circulation conduit; 7-a third circulation conduit; 8-a first connection pipe; 9-a second connecting tube; 10-a third connecting tube; 11-a motor; 12-21274; a handle; 13-a pin shaft; 14-a limiting rod; 16-a strut; 17-a support plate; 18-a gear motor; 19-a housing; 20-upper support; 21-a support plate; 22-a spring; 23-a limit bar; 24-a first slide bar; 25-a second slide bar; 26-a third slide bar; 27-closing plate; 28-a buffer tank; 29-a piston plate; 30-a piston rod; 31-a discharge pipe; 32-a material guide pipe; 33-a second valve; 34-a connecting shaft; 35-horizontal support plate; 36-a second feed port; 37-a first runner; 38-a second runner; 39-transverse limit groove.
Detailed Description
The present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
As shown in fig. 1-8, the invention provides an extraction device for heavy metal detection pretreatment in Tibetan medicinal materials, which is used for extracting a Tibetan medicinal digestion solution, and comprises:
the support comprises a lower support 1 and an upper support 20 which are in telescopic connection, wherein the upper support 20 is a pair of symmetrically arranged inverted L-shaped supports, the lower support 1 is a pair of oppositely arranged v-21274, the downward ends of the two inverted L-shaped supports are sleeved at the two v-21274, the ends of the two inverted L-shaped supports close to the outer side of the v-shaped supports are provided with matched pin holes, and the upper support 20 and the lower support 1 are in telescopic connection through a pin shaft 13 penetrating through the pin holes;
the reagent tank group is arranged on the upper bracket 20, and specifically, the reagent tank group is arranged between the two inverted L-shaped brackets and is fixedly connected with the two inverted L-shaped brackets respectively; the reagent tank group comprises a plurality of reagent tanks 3 which are vertically arranged side by side, discharge holes are formed in the bottoms of the reagent tanks 3, the number of the reagent tanks is a natural number which is more than two, and can be three, four, five, six, seven or eight, and the like, reagents in the reagent tanks can be Tibetan medicine digestion liquid, extracting agents and other pH regulators or inorganic salts, wherein the extracting agents can be single extracting agents or multiple extracting agents which are uniformly mixed, and corresponding extracting agents are selected according to extracted heavy metals; the extraction pipe group is arranged on the lower support 1, specifically, the extraction pipe group is arranged between two \ 21274 | -shaped supports and comprises a plurality of extraction pipes 2 which are vertically arranged side by side, a feed inlet is arranged at the top of each extraction pipe 2, a bottom discharge outlet is arranged at the bottom of each extraction pipe, matched and detachable covers are arranged at the feed inlet and the bottom discharge outlet, the detachable covers can be screwed or clamped, the adjacent extraction pipes 2 are fixedly connected through a connecting shaft 34, the adjacent extraction pipes are separated through a partition plate, the connecting shaft penetrates through the partition plate to be rotatably connected with the partition plate, and outward connecting shafts on the two outermost extraction pipes are respectively rotatably connected with the two \\\ 21274 | -shaped supports; the extraction pipe group drives the connecting shaft to operate through a motor 11, specifically, the output end of the motor 11 is provided with a speed reducing motor 18, and the output end of the speed reducing motor 18 is connected with the extraction pipe to drive the extraction pipe to operate; the motor 11 and the reducing motor 18 are both arranged on one of the 21274; the bracket through a supporting plate 17; the end part of the outermost connecting shaft far away from the motor 11 is fixedly connected with a limiting rod 14 and is close to the v-21274of the limiting rod 14, a support rod 16 for clamping the limiting rod 14 is arranged on the bracket, a clamping groove is arranged on the support rod 16, and the limiting rod 14 can be clamped in the clamping groove; scales are arranged on the outer wall of the extraction tube 2 and used for judging the amount of the added reagent;
a fluid guide group which is arranged between the reagent tank group and the extraction tube group and communicates the reagent tank group and the extraction tube group; the fluid diversion set comprises a pipeline conveying device and an overflow prevention device; pipeline conveyor sets up the below of reagent jar group, it includes a plurality of first pipelines and second pipeline, and a first pipeline passes through a reagent jar of discharge gate intercommunication in order to flow a reagent, be equipped with first valve 4 on the first pipeline, the second pipeline includes integrated into one piece's horizontal trunk line, a plurality of vertical small transfer line, trunk line, small transfer line all include the body that a plurality of coaxial sleeves were established, form the independent annular flow space of a plurality of reagents, a plurality of annular flow space of trunk line communicate with a plurality of first pipelines respectively, and the lower extreme of every small transfer line forms the discharge end of a plurality of reagents, and as shown in the figure, the body quantity that first pipeline, horizontal trunk line and vertical small transfer line cover were established is unanimous with the quantity of reagent jar, and E shape pipeline has been constituteed to horizontal trunk line and vertical small transfer line, and first circulation pipeline 5 has been constituteed respectively to each first pipeline and corresponding E-shaped pipeline, The second diversion pipeline 6 and the third diversion pipeline 7 are positioned on the horizontal main pipeline of the Nth layer according to the sleeving sequence of the horizontal main pipelines, the first pipeline connected with the second diversion pipeline is provided with N-1 connecting pipes for reagent circulation sleeved in the N-1 horizontal main pipelines on the horizontal main pipeline of the Nth layer, each connecting pipe corresponds to one horizontal main pipeline, as shown in the figure, the first diversion pipeline 5 is positioned on the outermost layer, the second diversion pipeline 6 is positioned on the innermost layer, the third diversion pipeline 7 is positioned on the middle layer, the second diversion pipeline 6 is provided with a first connecting pipe 8 and a third connecting pipe 10 for reagent circulation in the first diversion pipeline 5 and the third diversion pipeline 7, and the third diversion pipeline 7 is provided with a second connecting pipe 9 for reagent circulation in the first diversion pipeline 5; the lower end of each branch pipeline is communicated with an extraction pipe 2 through an overflow prevention device; the over-current prevention device is arranged above the extraction tube 2 and is detachably connected with the extraction tube, the detachable connection mode can be screw connection or clamping connection, and the over-current prevention device comprises a shell 19, a plurality of support plates 21, a plurality of adjusting structures and a clamping and blocking structure; the top of the shell is provided with a second feed port 36, the top of the shell 19 is detachably connected with the branch pipelines, specifically, the diameter of the second feed port 36 is consistent with the inner diameter of one vertical branch pipeline at the outermost periphery, the end face of each vertical branch pipeline is provided with a plurality of clamping ends, the outer edge of the second feed port 36 is provided with a plurality of clamping grooves matched with the clamping ends, and the detachable connection of the shell and the branch pipelines is realized through the clamping of the clamping ends and the clamping grooves; an adjusting structure is arranged on the shell 19 through a support plate 21, the number of the adjusting structure and the number of the support plate can be two, three, four, etc., the support plate 21 is a vertical support plate, a vertical first sliding groove 37 and a transverse limiting groove 39 communicated with the first sliding groove 37 are arranged on the support plate, the shape of the transverse limiting groove can be fan-shaped or v-21274, the transverse limiting groove and the first sliding groove are both made of elastic materials, the position where the transverse limiting groove is connected with the first sliding groove is an opening, the height of the opening is smaller than the diameter of a limiting rod, and the limiting rod can pass through the opening and be clamped in the transverse limiting groove; the adjusting structure comprises a plurality of coaxially sleeved slide bars vertically penetrating through the shell, a limiting rod 23 is arranged on the outer side of each slide bar, a second sliding groove 38 for the limiting rod 23 of one slide bar in the sliding structure to slide up and down is arranged on each slide bar, the limiting rods 23 sleeved with the slide bars from outside to inside are clamped in transverse limiting grooves 39 with different heights from top to bottom, the number of the slide bars in each adjusting structure is consistent with that of the branch pipelines, and as shown in the figure, a first slide bar 24, a second slide bar 25 and a third slide bar 26 are sequentially arranged according to the sleeving sequence from outside to inside; the blocking structure comprises a plurality of sealing plates 27 for blocking the discharge ends of a plurality of reagents of the branch pipelines, the sealing plate at the lowest part is in a circular structure, the sealing plate 27 above the sealing plate is in an annular structure with sequentially increasing outer diameters from bottom to top, one side of each sealing plate 27 is fixedly connected with the bottom of one sliding rod, namely, one side of each sealing plate 27 is connected with one sliding rod on one adjusting mechanism;
the spacing of the transverse limiting grooves 39 is set as follows: when the height of one limiting rod 23 is raised to enable the sealing plate 27 to be located at the preset height, the discharge end of one reagent of the branch pipeline is sealed;
in the technical scheme, in the use process, firstly, according to the principle that the sleeving sequence of the pipe bodies from outside to inside corresponds to the adding sequence of each reagent, each reagent is poured into a corresponding reagent tank, then the cover body at the feed inlet at the top of the extraction pipe is detached, the over-flow prevention device is arranged on the extraction pipe, each limit rod is sequentially clamped in the transverse limit groove according to the sleeving sequence of the slide rods from outside to inside, and the height is sequentially reduced; then the pin shaft for fixing the upper bracket and the lower bracket is drawn out, the upper bracket is moved downwards until each branch pipeline is clamped with the periphery of the second feed inlet of the overflow-preventing device, then the pin shaft is inserted, after the upper bracket and the lower bracket are fixed, the first valve on the first pipeline where the outermost pipe body is positioned is opened, the reagent in the reagent tank flows to each extraction pipe, the volume of the reagent in each extraction pipe is observed, when the reagent in a certain extraction pipe reaches the target volume, the highest limiting rod in the overflow-preventing device is moved into the first chute from the transverse limiting groove until the discharge end of the reagent in the branch pipeline is sealed by an annular sealing plate with the largest outer diameter, then the limiting rod is clamped in the corresponding transverse limiting groove, then the reagent volume in the rest extraction pipes is observed, when the reagent reaches the target volume, the highest limiting rod is moved into the first chute from the transverse limiting groove, closing the discharge end of the reagent, closing the first valve after the reagents in all the extraction tubes reach the target volume, opening the first valve on the first pipeline where the tube body sleeved on the layer 2 is located, and repeating the operation until all the reagents are added; after all reagents are added, the anti-overflow device is taken down from the extraction tube, the cover body of the feed port is arranged at the top of the extraction tube, then the motor and the speed reduction motor are started, the extraction tube starts to rotate under the action of the motor and the speed reduction motor, when the extraction time is up, the motor and the speed reduction motor are closed, the limiting rod is clamped on the support rod, standing is carried out for liquid layering in the extraction tube, then the discharge port is opened, and the target extraction liquid is collected;
by adopting the technical scheme, the reagent tank group and the pipeline conveying device are designed, so that an independent circulation space is provided for each reagent raw material, and the problems of pollution, volatilization and the like of the reagent in the transfer process are avoided; by designing the over-current prevention device, under the condition that the time for reagents to enter different extraction tubes is inconsistent, the discharge end where the reagent which preferentially reaches the target volume is located can be closed by using the blocking structure, so that test errors caused by different feeding amounts due to the inconsistent time for the reagents to enter the extraction tubes at different discharge ends are avoided; by designing the motor and the extraction pipe group, a plurality of parallel samples can be prepared simultaneously, and the extraction efficiency is improved; the method for extracting the heavy metal from the digestion solution of the Tibetan medicine can improve the efficiency and the accuracy of the subsequent detection of the heavy metal of the Tibetan medicine.
In another technical scheme, a horizontal support plate 35 is fixedly connected to the top of each support plate 21, and the horizontal support plate 35 faces the sliding rod; each limit rod 23 is fixedly connected with the horizontal support plate 35 through a spring 22; when the limiting rod 23 is clamped in the transverse limiting groove 39, the spring 22 is in a stretching state; in the technical scheme, in the use process, when the reagent in one extraction tube reaches the target volume, the corresponding limiting rod is moved to the first sliding groove from the transverse limiting groove, and the limiting rod drives the sliding rod and the sealing plate to move upwards under the action of the spring to seal the corresponding reagent discharging end; by adopting the technical scheme, the obtained beneficial effects are that, through designing horizontal support plate and spring, when moving the spacing stick to the first chute, under the effect of spring, the shrouding that can drive the slide bar bottom upwards moves, convenient operation, it is efficient.
In another technical scheme, the device further comprises a discharging mechanism, wherein the discharging mechanism comprises a discharging pipe 31 detachably connected with the bottom of the extraction pipe 2, the detachable connection mode can be clamping connection or screw connection, the section of the discharging pipe 31 can be square or round, a material guiding pipe 32 penetrating through the outer wall of the discharging pipe 31, and a buffer tank 28 fixedly connected with the free end part of the material guiding pipe 32; a liquid outlet pipe communicated with the buffer tank 28 is arranged at the bottom of the buffer tank 28, and a valve is arranged at the liquid outlet pipe and is a second valve 33; a piston plate 29 which is connected with the inner wall of the discharge pipe 31 in a sealing and sliding manner is arranged inside the discharge pipe 31, a piston rod 30 is arranged on one surface, away from the extraction pipe 2, of the piston plate 29, and the piston plate 29 moves up and down along the discharge pipe 31 to control the discharge flow rate of the discharge pipe 31; in the technical scheme, in the using process, after the extraction pipes are layered, the cover body of the discharge hole at the bottom of the extraction pipe is detached, the discharge pipe is installed, then the piston plate is moved, the discharge speed is controlled to be in the optimal state, the second valve is opened, and the target extraction liquid is collected; by adopting the technical scheme, the beneficial effects are that the discharging speed of the target extraction liquid can be effectively controlled by designing the piston plate, the piston rod, the material guide pipe, the liquid outlet and the valve when the target extraction liquid is collected; through designing the buffer tank, can let the target extraction liquid that flows out carry out the buffer through the buffer tank, avoid the extraction liquid velocity of flow too fast to cause the separation effect poor, improve follow-up heavy metal detection test's accuracy nature.
In another technical scheme, a lifting handle 12 is arranged above the reagent pot group, and the two ends of the lifting handle 12 in the same direction are fixedly connected with the upper bracket 20; by adopting the technical scheme, the utility model has the beneficial effects that the upper bracket can be conveniently taken by designing the 21274-shaped handle on the upper bracket, and the practicability of the device is improved.
In another technical scheme, the outer surface of the sealing plate is coated with a sealing layer, and the sealing layer can be made of rubber or silica gel; by adopting the technical scheme, the obtained beneficial effect is that the test error caused by the fact that redundant reagents flow into the extraction tube is effectively prevented by coating the sealing layer on the outer surface of the sealing plate.
< example 1>
An extraction method for detection pretreatment of heavy metals in Tibetan medicinal materials is characterized in that an extraction device for detection pretreatment of heavy metals in Tibetan medicinal materials is adopted to extract digestion liquid of the Tibetan medicinal materials; the extraction device for heavy metal detection preliminary treatment in Tibetan medicinal material includes:
the support comprises a lower support 1 and an upper support 20 which are in telescopic connection, wherein the upper support 20 is a pair of symmetrically arranged inverted L-shaped supports, the lower support 1 is a pair of oppositely arranged v-21274, the downward ends of the two inverted L-shaped supports are sleeved at the two v-21274, the ends of the two inverted L-shaped supports close to the outer side of the v-shaped supports are provided with matched pin holes, and the upper support 20 and the lower support 1 are in telescopic connection through a pin shaft 13 penetrating through the pin holes;
the reagent tank group is arranged on the upper bracket 20, and specifically, the reagent tank group is arranged between the two inverted L-shaped brackets and is fixedly connected with the two inverted L-shaped brackets respectively; the reagent tank group comprises a plurality of reagent tanks 3 which are vertically arranged side by side, discharge holes are formed in the bottoms of the reagent tanks 3, the number of the reagent tanks is a natural number which is more than two, and can be three, four, five, six, seven or eight, and the like, reagents in the reagent tanks can be Tibetan medicine digestion liquid, extracting agents and other pH regulators or inorganic salts, wherein the extracting agents can be single extracting agents or multiple extracting agents which are uniformly mixed, and corresponding extracting agents are selected according to extracted heavy metals; the extraction pipe group is arranged on the lower support 1, specifically, the extraction pipe group is arranged between two \ 21274 | -shaped supports and comprises a plurality of extraction pipes 2 which are vertically arranged side by side, a feed inlet is arranged at the top of each extraction pipe 2, a bottom discharge outlet is arranged at the bottom of each extraction pipe, matched and detachable covers are arranged at the feed inlet and the bottom discharge outlet, the detachable covers can be screwed or clamped, the adjacent extraction pipes 2 are fixedly connected through a connecting shaft 34, the adjacent extraction pipes are separated through a partition plate, the connecting shaft penetrates through the partition plate to be rotatably connected with the partition plate, and outward connecting shafts on the two outermost extraction pipes are respectively rotatably connected with the two \\\ 21274 | -shaped supports; the extraction pipe group drives the connecting shaft to operate through a motor 11, specifically, the output end of the motor 11 is provided with a speed reducing motor 18, and the output end of the speed reducing motor 18 is connected with the extraction pipe to drive the extraction pipe to operate; the motor 11 and the reducing motor 18 are both arranged on one of the 21274; the bracket through a supporting plate 17; the end part of the outermost connecting shaft far away from the motor 11 is fixedly connected with a limiting rod 14 and is close to the v-21274of the limiting rod 14, a support rod 16 for clamping the limiting rod 14 is arranged on the bracket, a clamping groove is arranged on the support rod 16, and the limiting rod 14 can be clamped in the clamping groove; scales are arranged on the outer wall of the extraction tube 2 and used for judging the amount of the added reagent, or a weight sensor is arranged at the bottom of the extraction tube and used for judging the weight of the added reagent;
a fluid guide group which is arranged between the reagent tank group and the extraction tube group and communicates the reagent tank group and the extraction tube group; the fluid diversion set comprises a pipeline conveying device and an overflow prevention device; pipeline conveyor sets up the below of reagent tank group, it includes a plurality of first pipelines and second pipeline, and a first pipeline passes through a reagent tank of discharge gate intercommunication in order to flow a reagent, be equipped with first valve 4 on the first pipeline, the second pipeline includes integrated into one piece's horizontal trunk line, a plurality of vertical small transfer line, trunk line, small transfer line all include the body that a plurality of coaxial sleeves were established, form the independent annular flow space of a plurality of reagents, a plurality of annular flow space of trunk line communicate with a plurality of first pipelines respectively, and the lower extreme of every small transfer line forms the discharge end of a plurality of reagents, and as shown in the figure, the body quantity that first pipeline, horizontal trunk line and vertical small transfer line cover were established is unanimous with the quantity of reagent tank, and horizontal trunk line and vertical small transfer line have constituteed E shape pipeline, and first circulation pipeline 5 has been constituteed respectively to every first pipeline and the corresponding E-shaped pipe, The second diversion pipeline 6 and the third diversion pipeline 7 are positioned on the horizontal main pipeline of the Nth layer according to the sleeving sequence of the horizontal main pipelines, the first pipeline connected with the second diversion pipeline is provided with N-1 connecting pipes for reagent circulation sleeved in the N-1 horizontal main pipelines on the horizontal main pipeline of the Nth layer, each connecting pipe corresponds to one horizontal main pipeline, as shown in the figure, the first diversion pipeline 5 is positioned on the outermost layer, the second diversion pipeline 6 is positioned on the innermost layer, the third diversion pipeline 7 is positioned on the middle layer, the second diversion pipeline 6 is provided with a first connecting pipe 8 and a third connecting pipe 10 for reagent circulation in the first diversion pipeline 5 and the third diversion pipeline 7, and the third diversion pipeline 7 is provided with a second connecting pipe 9 for reagent circulation in the first diversion pipeline 5; the lower end of each branch pipeline is communicated with an extraction pipe 2 through an overflow prevention device; the over-current prevention device is arranged above the extraction pipe 2 and is detachably connected with the extraction pipe, the detachable connection mode can be a screw connection or a clamping connection, and the over-current prevention device comprises a shell 19, a plurality of support plates 21, a plurality of adjusting structures and a blocking structure; the top of the shell is provided with a second feed port 36, the top of the shell 19 is detachably connected with the branch pipelines, specifically, the diameter of the second feed port 36 is consistent with the inner diameter of one vertical branch pipeline at the outermost periphery, the end face of each vertical branch pipeline is provided with a plurality of clamping ends, the outer edge of the second feed port 36 is provided with a plurality of clamping grooves matched with the clamping ends, and the detachable connection of the shell and the branch pipelines is realized through the clamping of the clamping ends and the clamping grooves; an adjusting structure is arranged on the shell 19 through a support plate 21, the number of the adjusting structure and the number of the support plate can be two, three, four, etc., the support plate 21 is a vertical support plate, a vertical first sliding groove 37 and a transverse limiting groove 39 communicated with the first sliding groove 37 are arranged on the support plate, the shape of the transverse limiting groove can be fan-shaped or v-21274, the transverse limiting groove and the first sliding groove are both made of elastic materials, the position where the transverse limiting groove is connected with the first sliding groove is an opening, the height of the opening is smaller than the diameter of a limiting rod, and the limiting rod can pass through the opening and be clamped in the transverse limiting groove; the adjusting structure comprises a plurality of coaxially sleeved slide bars vertically penetrating through the shell, a limiting rod 23 is arranged on the outer side of each slide bar, a second sliding groove 38 for the limiting rod 23 of one slide bar in the sliding structure to slide up and down is arranged on each slide bar, the limiting rods 23 sleeved with the slide bars from outside to inside are clamped in transverse limiting grooves 39 with different heights from top to bottom, the number of the slide bars in each adjusting structure is consistent with that of the branch pipelines, and as shown in the figure, a first slide bar 24, a second slide bar 25 and a third slide bar 26 are sequentially arranged according to the sleeving sequence from outside to inside; the blocking structure comprises a plurality of sealing plates 27 for blocking the discharge ends of a plurality of reagents of the branch pipelines, the sealing plate at the lowest part is in a circular structure, the sealing plate 27 above the sealing plate is in an annular structure with sequentially increasing outer diameters from bottom to top, one side of each sealing plate 27 is fixedly connected with the bottom of one sliding rod, namely, one side of each sealing plate 27 is connected with one sliding rod on one adjusting mechanism;
the spacing of the transverse limiting grooves 39 is set as follows: when the height of one limiting rod 23 is raised to enable the sealing plate 27 to be located at the preset height, the discharge end of one reagent of the branch pipeline is sealed;
in this embodiment, cloud point extraction is adopted to extract the digestion solution of the Tibetan medicine material, the Tibetan medicine material is one of Tibetan medicines such as cordyceps sinensis, snow lotus herb, rhodiola rosea and saffron crocus, and mainly lead in the Tibetan medicine material is extracted and enriched, the reagent used in this embodiment includes fatty alcohol polyoxyethylene ether, 10 μ L/mL schiff base, pH value regulator, ammonium sulfate and deionized water, the fatty alcohol polyoxyethylene ether is a nonionic surfactant, the schiff base is used as a ligand, the schiff base mainly refers to a class of compounds containing imine or an imine group, the schiff base is synthesized by o-phenylenediamine and salicylaldehyde in this embodiment, the pH value regulator can be a phosphoric acid buffer solution, and the specific extraction steps are as follows:
s1, adding reagent into the reagent tank, wherein the over-current prevention device is in place; specifically, according to the principle that the sleeving sequence of the tube body from outside to inside corresponds to the adding sequence of each reagent, each reagent is poured into a corresponding reagent tank, then the cover body at the feed inlet at the top of the extraction tube is detached, the over-current prevention device is installed on the extraction tube, and each limiting rod is sequentially clamped in the transverse limiting groove according to the sleeving sequence of the sliding rods from outside to inside, and the heights are sequentially decreased; in this embodiment, the raw materials and the reagents in the reagent tank are sequentially added in the order of: 5ml of Tibetan medicine digestion solution, 100 Schiff base reagent and 200 mu L, pH value regulator, 100 fatty alcohol-polyoxyethylene ether reagent and 200 mu L of ammonium sulfate reagent, 0.5-1.0g of deionized water, wherein the pH value of the solution is regulated to about 7.0 by using the pH value regulator, and the solution is diluted to 10ml by using the deionized water;
s2, adding the reagent in the S1 to the extraction tube through the fluid diversion group; specifically, the pin shaft for fixing the upper support and the lower support is pulled out, the upper support is moved downwards to each branch pipeline to be clamped with the periphery of a second feed inlet of the overflow prevention device, then the pin shaft is inserted, after the upper support and the lower support are fixed, a first valve on a first pipeline where an outermost pipe body is located is opened, a reagent in a reagent tank flows to each extraction pipe, the volume of the reagent in each extraction pipe is observed, after the reagent in a certain extraction pipe reaches a target volume or a target weight, a highest limiting rod in the overflow prevention device is moved into a first sliding groove from a transverse limiting groove until an annular sealing plate with the largest outer diameter seals a discharge end of the reagent in the branch pipeline, then the limiting rod is clamped in the corresponding transverse limiting groove, then the reagent volume in the rest extraction pipes is observed, and after the reagent reaches the target volume, the highest limiting rod is moved into the first sliding groove from the transverse limiting groove, closing the discharge end of the reagent, closing the first valve after the reagents in all the extraction tubes reach the target volume, opening the first valve on the first pipeline where the tube body sleeved on the layer 2 is located, and repeating the operation until all the reagents are added;
s3, starting the motor, rotating the extraction tube in S2, extracting for 5-10min, and collecting target extraction liquid; specifically, after all reagents are added, the anti-overflow device is taken down from the extraction tube, the cover body of the feeding hole is installed at the top of the extraction tube, then the motor and the speed reduction motor are started, the extraction tube starts to rotate under the action of the motor and the speed reduction motor, the extraction time is 5-10min, after the extraction time is reached, the motor and the speed reduction motor are closed, the limiting rod is clamped on the supporting rod, standing is carried out for liquid layering in the extraction tube, then the discharging hole is opened, and the target extraction liquid is collected.
The number of apparatuses and the scale of the process described herein are intended to simplify the description of the present invention. The application, modification and variation of the extraction method and the extraction device for the heavy metal detection pretreatment in Tibetan medicines of the invention are obvious to those skilled in the art.
While embodiments of the invention have been described above, it is not intended to be limited to the details shown, described and illustrated herein, but is to be accorded the widest scope consistent with the principles and novel features herein disclosed, and to such extent that such modifications are readily available to those skilled in the art, and it is not intended to be limited to the details shown and described herein without departing from the general concept as defined by the appended claims and their equivalents.

Claims (7)

1. Extraction element for heavy metal detection preliminary treatment in Tibetan medicinal material for extract Tibetan medicinal material digestion liquid, its characterized in that includes:
the support comprises a lower support and an upper support which are connected in a telescopic manner;
the reagent tank group is arranged on the upper bracket and comprises a plurality of reagent tanks which are vertically arranged side by side, and a discharge hole is formed in the bottom of each reagent tank; the extraction pipe group is arranged on the lower bracket and comprises a plurality of extraction pipes which are vertically arranged side by side, adjacent extraction pipes are fixedly connected through a connecting shaft, and the extraction pipe group is driven by a motor to operate; scales are arranged on the outer wall of the extraction tube;
a fluid guide group which is arranged between the reagent tank group and the extraction tube group and communicates the reagent tank group and the extraction tube group; the fluid diversion set comprises a pipeline conveying device and an overflow prevention device; the pipeline conveying device is arranged below the reagent tank group and comprises a plurality of first pipelines and second pipelines, one first pipeline is communicated with one reagent tank through the discharge port to flow one reagent, the second pipeline comprises a horizontal main pipeline and a plurality of vertical branch pipelines which are integrally formed, the main pipeline and the branch pipelines respectively comprise a plurality of pipe bodies which are coaxially sleeved to form independent annular flowing spaces of the plurality of reagents, the plurality of annular flowing spaces of the main pipeline are respectively communicated with the plurality of first pipelines, and the lower end of each branch pipeline forms the discharge end of the plurality of reagents; the lower end of each branch pipeline is communicated with an extraction pipe through an overflow prevention device; the anti-overflow device is arranged above the extraction tube and comprises a shell, a plurality of support plates, a plurality of adjusting structures and a blocking structure; the top of the shell is detachably connected with the branch pipeline, an adjusting structure is arranged on the shell through a support plate, and the support plate is provided with a vertical first chute and a transverse limiting groove communicated with the first chute; the adjusting structure comprises a plurality of coaxially sleeved slide bars vertically penetrating through the shell, a limiting rod is arranged on the outer side of each slide bar, a second sliding groove for the limiting rod of one slide bar in the slide bar to slide up and down is formed in each slide bar, and the limiting rods sleeved with the slide bars from outside to inside are clamped in the transverse limiting grooves at different heights from top to bottom; the blocking structure comprises a plurality of sealing plates for blocking the discharge ends of a plurality of reagents of the branch pipelines, the sealing plate at the lowest part is of a circular structure, the sealing plate above the circular structure is of an annular structure with sequentially increasing outer diameters from bottom to top, and one side of each sealing plate is fixedly connected with the bottom of one sliding rod;
the interval of horizontal spacing groove sets up to: when the height of a limiting rod is increased to enable the sealing plate to be located at the preset height, the discharge end of a reagent of the branch pipeline is sealed.
2. The extraction device for detecting and pretreating heavy metals in Tibetan medicines according to claim 1, wherein a horizontal support plate is fixedly connected to the top of each support plate, and the horizontal support plate faces the slide bar; each limit rod is fixedly connected with the horizontal support plate through a spring; when the limiting rod is clamped in the transverse limiting groove, the spring is in a stretching state.
3. The extraction device for detecting and pretreating heavy metals in Tibetan medicines according to claim 1, further comprising a discharging mechanism, wherein the discharging mechanism comprises a discharging pipe detachably connected with the bottom of the extraction pipe, a material guiding pipe penetrating through the outer wall of the discharging pipe, and a buffer tank fixedly connected with the free end part of the material guiding pipe; a liquid outlet is formed in the bottom of the buffer tank, and a valve is arranged at the liquid outlet; the device is characterized in that a piston plate in sliding connection with the inner wall of the discharging pipe in a sealing mode is arranged inside the discharging pipe, the height of the piston plate is the same as the diameter of the liquid outlet, a piston rod is arranged on one face, away from the extraction pipe, of the piston plate, the piston plate moves up and down along the discharging pipe, and the discharging flow rate of the discharging pipe is controlled.
4. The extraction device for the detection and pretreatment of heavy metals in Tibetan medicines as claimed in claim 3, wherein the cross section of the discharge pipe is square.
5. The extraction device for detecting and pretreating heavy metals in Tibetan medicines according to claim 1, wherein a v-21274 '-shaped handle is arranged above the reagent tank group, and two ends of the v-21274' -shaped handle in the same direction are fixedly connected with the upper support.
6. The extraction device for detecting and pretreating heavy metals in Tibetan medicines as claimed in claim 1, wherein a sealing layer is coated on the outer surface of the sealing plate.
7. The extraction method for the detection pretreatment of the heavy metals in the Tibetan medicinal materials is characterized in that the extraction device for the detection pretreatment of the heavy metals in the Tibetan medicinal materials as claimed in any one of claims 1 to 6 is adopted to extract the digestion solution of the Tibetan medicinal materials, and the specific steps are as follows:
s1, adding reagent into the reagent tank, wherein the over-current prevention device is in place;
s2, adding the reagent in the S1 into the extraction tube through the fluid diversion group;
and S3, starting the motor, rotating the extraction tube in the S2, extracting for 5-10min, and collecting the target extraction liquid.
CN202110089746.4A 2021-01-22 2021-01-22 Extraction method and extraction device for heavy metal detection pretreatment in Tibetan medicinal materials Active CN112915584B (en)

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