CN113960207A - Semi-solid preparation pharmaceutical analytical determination method based on HPLC - Google Patents
Semi-solid preparation pharmaceutical analytical determination method based on HPLC Download PDFInfo
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- CN113960207A CN113960207A CN202111254762.0A CN202111254762A CN113960207A CN 113960207 A CN113960207 A CN 113960207A CN 202111254762 A CN202111254762 A CN 202111254762A CN 113960207 A CN113960207 A CN 113960207A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/36—Control of physical parameters of the fluid carrier in high pressure liquid systems
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Abstract
The invention discloses an analytical determination method for semisolid preparation medicines based on HPLC, which relates to the technical field of medicine analysis and comprises the following steps: pretreatment for measurement, preparation of analysis measurement solution, screening of preparation residues, accurate sampling, chromatographic conditions and measurement on a computer. According to the invention, the injection barrel is arranged on the rack, and a small amount of residual solution to be measured attached to the lower part of the extraction channel can be blown under the action of cold hot air in the vortex tube, so that the measurement error caused by the loss of the dose of the solution to be measured is avoided, and the mounting position of the bolt is adjusted according to the accurate debugging scale on the rotating part, so that the solution to be measured with accurate quantitative proportion can be controlled; the output shaft of the driving motor drives the cam to rotate, so that trace solid dosage preparation residues in the semisolid preparation are filtered, and frequent blockage of a chromatographic column in an HPLC instrument is avoided.
Description
Technical Field
The invention relates to the technical field of drug analysis, in particular to an analytical determination method for a semisolid preparation drug based on HPLC.
Background
At present, pharmacological activities of pulsatilla chinensis bunge medicines are researched more, the existing quality research aspect aims at researching pulsatilla chinensis bunge saponins, and the method mainly comprises the steps of measuring the content of pulsatilla chinensis bunge saponins in different pulsatilla chinensis bunge, researching the content of pulsatilla chinensis bunge saponins in different producing areas and the like, and the analysis method for measuring the saponin and other components of the semi-solid preparation medicines is generally adopted by dissolving and separating out the pulsatilla chinensis bunge saponins, and then directly measuring the separated and dissolved solution by HPLC.
However, in the long-term analysis and measurement process in the prior art, certain disadvantages are found to exist: firstly, because the semisolid preparation has certain viscosity, the semisolid preparation is very easy to adhere to a sampling device in the sampling process, so that accurate quantitative proportioning cannot be realized, and a sampling mode of measuring dissolved measuring liquid is adopted, so that a small amount of the measuring dissolving liquid still adheres to the sampling device, a certain deviation occurs in a measuring result, the dosage of the sampling device is fixed, and if the analysis and measurement quantity of the dissolving liquid to be measured is changed greatly, the corresponding device needs to be replaced, so that the universality is poor; secondly, the semisolid preparation contains a certain amount of solid dosage preparation residues, and the phenomenon of chromatographic column blockage often occurs in the process of directly analyzing and determining for many times on an HPLC instrument, so that the replacement cost is high, and time and labor are consumed.
Disclosure of Invention
The invention aims to provide an analytical determination method for semisolid preparations based on HPLC (high performance liquid chromatography), which aims to solve the defects caused by the prior art.
An analytical assay method for pharmaceutical use of semi-solid formulations based on HPLC comprising the steps of:
s1: pretreatment for measurement: taking a proper amount of semisolid preparation medicine to be measured, putting the semisolid preparation medicine into the charging barrel body and installing the charging barrel body on the rack;
s2: preparation of analytical measurement solution: dissolving the sample with methanol and acetonitrile single solvent or methanol-water, acetonitrile-water, methanol-acid and alkali, methanol-acid and acid ammonium salt water solution to extract multiple saponin components;
s3: the formulation residue was sieved and sampled accurately: screening residues of the dissolved solution by a sampling mechanism arranged on a rack, filtering tiny solid residues, vibrating powder of the filtered dissolved solution at low temperature, sampling by accurate quantitative proportion, heating for a short time, flowing out of a measuring solution, and blowing off;
s4: chromatographic conditions are as follows: the chromatographic column is a reversed-phase chromatographic column, and the reversed-phase chromatographic column is selected from a phenyl silane bonded silica gel chromatographic column, an octadecyl silane bonded silica gel chromatographic column or an octaalkyl silane bonded silica gel chromatographic column;
taking a mixed solution of acid and alkali or acid and ammonium salt aqueous solution and an organic phase as a mobile phase, wherein the pH value of a water phase ranges from 2 to 8, and the organic phase is methanol or acetonitrile; performing gradient elution by adopting an isocratic or gradient elution method, wherein the volume ratio of the water phase in the mobile phase in isocratic elution is 90-60%, the ratio of the mobile phase in gradient elution is at time points of 0, 20-30, 32-35 and 36-45 min, and the volume ratio of the water phase is 80-75%, 20-30% and 20-80%;
s5: testing on a machine: and (4) injecting the analysis solution prepared in the step S3 into an HPLC instrument, performing chromatographic analysis, and recording a chromatogram.
Preferably, the upper end of the rack is fixedly provided with a material collecting frame, and a liquid supply pump communicated to the inside of the sampling mechanism is installed at the side end of the material collecting frame.
Preferably, the sampling mechanism comprises a driving motor, an extraction channel and a vortex tube, the driving motor is installed on the frame through an installation frame, a cam is installed on an output shaft of the driving motor, a premixing barrel is installed at the upper end of the material collecting frame, a support piece is installed at the side end of the material collecting frame, a first push rod is arranged on the support piece in a sliding mode, a spring is sleeved between the end portion, close to one side of the cam, of the first push rod and the support piece, the other end of the first push rod is hinged to a second push rod, a flywheel is installed at the side end of the premixing barrel, the side end of the flywheel is eccentrically hinged to the other end of the second push rod, a stirring fan is coaxially installed in the premixing barrel and is provided with a vibration dispersing arm, the end portion of the driving motor penetrates through the support piece and is connected with the first rotating rod, the other end of the first rotating rod is hinged to a second rotating rod, and the outer end of the extraction channel is installed on the frame through the installation frame, draw the upper end of passageway to communicate in the lower part of premixing a section of thick bamboo through the filter plate, it is connected with the rotation portion to rotate on the mounting bracket, the middle part of rotation portion is articulated mutually with the other end of bull stick two through adjustable bolt, and the tip of rotation portion is provided with the top, and the middle part of drawing the passageway is provided with the stop valve, the vortex tube is installed in the side of mounting bracket, and the one end of vortex tube links to each other with the rotation portion through taking over one, and the other end of vortex tube is connected with the water conservancy diversion calandria through taking over two, the other end of water conservancy diversion calandria communicates in the lower part side of drawing the passageway.
Preferably, the inner bottom surface of the upper part of the extraction channel is hinged with a plurality of uniformly distributed material blocking magnetic plates.
Preferably, the rotating part is of a hollow structure, and the end part connected with the top head is matched with the side end surface of the extraction channel.
Preferably, the whole extraction channel is arranged in an inclined downward direction, and the lower inclined angle of the extraction channel is relatively larger than the upper inclined angle of the extraction channel.
Preferably, the guide discharging pipe is arranged obliquely downwards relative to the lower part of the extraction channel.
Preferably, the lower port of the extraction channel is connected to an HPLC instrument.
The invention has the advantages that:
(1) through arranging the material injection barrel on the frame and arranging the sampling mechanism and the liquid supply pump at the side end of the material collecting frame, a plurality of pulsatilla saponin components are extracted from the premixing barrel, the output end of the driving motor drives the rotating part to rotate on the vortex tube in a reciprocating way through the vibrating arm and the rotating rod, the upper part of the extraction channel is rapidly cooled to a solidification state by measuring the solution under the action of cold flow air in the vortex tube, the continuous vibrating and knocking of the vibrating arm on the extraction channel are matched, the measured solution is vibrated to be in an unequal particle state after being solidified, the vibrating powder measuring particles rapidly enter the lower part of the extraction channel with a larger inclination angle through the opening and closing action of the stop valve, the residual small amount of the measured solution attached to the lower part of the extraction channel can be blown under the action of the oblique hot flow air in the vortex tube, and the measuring error caused by the loss of the dose of the measured solution is avoided, the mounting position of the bolt is adjusted according to the accurate debugging scale on the rotating part, so that the measured solution with the required accurate quantitative proportion can be controlled;
(2) the output shaft through the driving motor drives the cam to rotate, the flywheel is driven to rotate through the first push rod and the second push rod, the stirring fan in the premixing cylinder is driven to stir the internal mixed liquid, solid dosage preparation residues are dissolved and rapidly separated out in an accelerated mode, the preparation residues are screened through the filter plate, the filtering of trace solid dosage preparation residues in the semisolid preparation is achieved, and frequent blockage of a chromatographic column in an HPLC instrument is avoided.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is a side view of the structure of the apparatus used in the present invention.
FIG. 3 is a schematic structural diagram of a sampling mechanism according to the present invention.
FIG. 4 is a schematic view of the internal structure of the sampling mechanism of the present invention.
Fig. 5 is an enlarged view of the structure at a in fig. 4.
FIG. 6 is a schematic diagram of the internal structure of the extraction channel of the present invention.
Fig. 7 is an assembly view of the rotating part, the bolt and the plug in the present invention.
The device comprises a material injection barrel, a 2-frame, a 3-sampling mechanism, a 4-material collecting frame, a 5-liquid supply pump, a 301-driving motor, a 302-extraction channel, a 303-vortex tube, a 304-mounting frame, a 305-cam, a 306-premixing barrel, a 307-supporting piece, a 308-push rod I, a 309-spring, a 310-push rod II, a 311-flywheel, a 313-stirring fan, a 314-vibration dispersion arm, a 315-rotating rod I, a 316-rotating rod II, a 317-fixing frame, a 318-filter plate, a 319-rotating part, a 320-bolt, a 321-top head, a 322-stop valve, a 323-connecting pipe I, a 324-connecting pipe II, a 325-flow guide discharge pipe and a 326-material blocking magnetic plate.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
As shown in fig. 1 to 7, an analytical assay method for pharmaceutical use of semisolid formulations based on HPLC comprises the following steps:
s1: pretreatment for measurement: taking a proper amount of semisolid preparation medicine to be measured, putting the semisolid preparation medicine into the material injection cylinder body 1 and installing the semisolid preparation medicine on the rack 2;
s2: preparation of analytical measurement solution: dissolving the sample with methanol and acetonitrile single solvent or methanol-water, acetonitrile-water, methanol-acid and alkali, methanol-acid and acid ammonium salt water solution to extract multiple saponin components;
s3: the formulation residue was sieved and sampled accurately: screening residues of the dissolved solution by a sampling mechanism 3 arranged on a frame 2, filtering micro solid residues, vibrating the filtered dissolved solution at low temperature, sampling by accurate quantitative proportion, heating for a short time, flowing out a measured solution, and blowing off the measured solution;
s4: chromatographic conditions are as follows: the chromatographic column is a reversed-phase chromatographic column, and the reversed-phase chromatographic column is selected from a phenyl silane bonded silica gel chromatographic column, an octadecyl silane bonded silica gel chromatographic column or an octaalkyl silane bonded silica gel chromatographic column;
taking a mixed solution of acid and alkali or acid and ammonium salt aqueous solution and an organic phase as a mobile phase, wherein the pH value of a water phase ranges from 2 to 8, and the organic phase is methanol or acetonitrile; performing gradient elution by adopting an isocratic or gradient elution method, wherein the volume ratio of the water phase in the mobile phase in isocratic elution is 90-60%, the ratio of the mobile phase in gradient elution is at time points of 0, 20-30, 32-35 and 36-45 min, and the volume ratio of the water phase is 80-75%, 20-30% and 20-80%;
s5: testing on a machine: and (4) injecting the analysis solution prepared in the step S3 into an HPLC instrument, performing chromatographic analysis, and recording a chromatogram.
In this embodiment, a material collecting frame 4 is fixedly disposed at the upper end of the frame 2, and a liquid feeding pump 5 communicated to the sampling mechanism 3 is installed at a side end of the material collecting frame 4.
In this embodiment, the sampling mechanism 3 includes a driving motor 301, an extraction channel 302 and a vortex tube 303, the driving motor 301 is installed on the frame 2 through an installation frame 304, a cam 305 is installed on an output shaft of the driving motor 301, a pre-mixing barrel 306 is installed at the upper end of the material collecting frame 4, a supporting member 307 is installed at the side end of the material collecting frame 4, a first push rod 308 is slidably installed on the supporting member 307, a spring 309 is sleeved between the end portion of the first push rod 308 close to one side of the cam 305 and the supporting member 307, a second push rod 310 is hinged to the other end of the first push rod 308, a flywheel 311 is installed at the side end of the pre-mixing barrel 306, the side end of the flywheel 311 is eccentrically hinged to the other end of the second push rod 310, a stirring fan 313 is coaxially installed in the pre-mixing barrel 306, a vibration dispersion arm 314 is coaxially installed at the other end of the pre-mixing barrel 306 and the stirring fan 313, the end portion of the driving motor 301 penetrates through the supporting member 307 and is connected with a first rotating rod 315, the other end of bull stick 315 articulates there is bull stick two 316, the outer end of drawing passageway 302 passes through mount 317 and installs in frame 2, draws the upper end of passageway 302 and passes through filter plate 318 and communicate in the lower part of premixing a section of thick bamboo 306, it has rotation portion 319 to rotate to be connected with on the mounting bracket 304, the middle part of rotation portion 319 is articulated mutually through the other end of adjustable bolt 320 with bull stick two 316, and the tip of rotation portion 319 is provided with top 321, and the middle part of drawing passageway 302 is provided with stop valve 322, vortex tube 303 is installed in the side of mounting bracket 304, and vortex tube 303's one end links to each other with rotation portion 319 through taking over a 323, and vortex tube 303's the other end is connected with water conservancy diversion calandria 325 through taking over two 324, the other end of water conservancy diversion calandria 325 communicates in the lower part side of drawing passageway 302.
It should be noted that driving motor 301 is servo motor, it has the striker plate 326 of a plurality of equipartition to articulate to draw the bottom surface in the upper portion of passageway 302, top 321 is permanent magnet structure, and the magnetism of top 321 and striker plate 326's magnetism inhale for opposite sex, and striker plate 326's height is not higher than the internal diameter of drawing passageway 302 for striker plate 326 does not contact with the inner wall of drawing passageway 302 at the in-process of upset, draws simultaneously on the passageway 302 with top 321 matched with side be the slot inlet structure.
In this embodiment, the rotating portion 319 has a hollow structure, and the end connected to the plug 321 is engaged with the side end surface of the extraction channel 302 to prevent cold fluid gas from being excessively sprayed out of the extraction channel 302, and a precise adjustment scale is provided on the rotating portion 319 at the position engaged with the bolt 320.
In this embodiment, the whole extraction channel 302 is arranged in an inclined downward direction, and the inclination angle of the lower part of the extraction channel 302 is relatively larger than the inclination angle of the upper part of the extraction channel 302, so that the assay preparation in a solid particle structure can roll down along the extraction channel 302 after the stop valve 322 is opened, and can be prevented from adhering to the inner wall of the extraction channel 302.
In this embodiment, the drainage pipe 325 is disposed in an obliquely downward direction with respect to the lower portion of the extraction channel 302, and is used to extract all the high-flow state measurement solution in cooperation with the obliquely incident high-speed airflow.
It should be noted that one end of the first communication connection pipe 323 on the vortex tube 303 is a cold flow end, and one end of the second communication connection pipe 324 is a hot flow end.
In addition, the lower port of the extraction channel 302 is connected to an HPLC instrument.
The working process and principle are as follows: in the using process, the invention carries out measurement pretreatment, preparation analysis and measurement solution, screening preparation residues and accurate sampling, chromatographic conditions and on-machine measurement in sequence according to working procedures, in the process of preparing analysis and measurement solution, screening preparation residues and accurate sampling, firstly, a semisolid preparation to be measured and a dissolving liquid are respectively filled into a premixing cylinder 306 through a material injection cylinder body 1 and a liquid supply pump 5 to dissolve a sample, a plurality of Chinese medicine semisolid pulsatilla saponin components in the Chinese medicine semisolid pulsatilla preparation are extracted, then, a driving motor 301 and a vortex tube 303 are simultaneously started, an output shaft of the driving motor 301 drives a cam 305 to rotate, then a flywheel 311 is driven to rotate through a first push rod 308 and a second push rod 310 to drive a stirring fan 313 in the premixing cylinder 306 to stir the internal mixed liquid so as to accelerate dissolution and rapidly separate out solid preparation residues, and then the preparation residues are screened through a filter plate 318, and discharged into the material collecting rack 4 below to prepare a filtered measuring solution which enters the extraction channel 302;
meanwhile, the output end of the driving motor 301 drives the rotating part 319 to rotate on the vortex tube 304 in a reciprocating manner through the vibration dispersion arm 315 and the second rotating rod 316, the top 321 at the end part is driven to turn over the material blocking magnetic plate 326 inside the extraction channel 302 upwards in the process that the rotating part 319 rotates towards the right side, at the moment, under the action of cold air in the vortex tube 303, the measured solution is rapidly cooled to a solidification state on the upper part of the extraction channel 302, the measured solution is vibrated to be in an uneven particle state after being solidified by matching with the continuous vibration and striking of the extraction channel 302 by the vibration dispersion arm 314, at the moment, the vibration powder measurement particles are concentrated at the lower parts of a plurality of material blocking magnetic plates 326, and in the process that the rotating part 319 rotates towards the left side, the material blocking magnetic plates 326 are driven to turn downwards, and the material blocking magnetic plates are driven to roll downwards by self gravity in the inclined extraction channel 302 under the driving of the air flow;
when the end of the rotating part 319 rotates to the position of the stop valve 322, the stop valve 322 is opened to enable the powder vibration measuring particles to rapidly enter the lower position of the extraction channel 302 with a larger inclination angle, the powder vibration measuring particles are rapidly melted to be molten under the action of hot air in the vortex tube 303, and a small amount of measuring solution attached to the lower part of the extraction channel 302 can be blown by matching with a plurality of air nozzles on the flow guide discharge pipe 325 which is obliquely arranged downwards until all the solution to be measured enters an HPLC instrument connected with the tail end of the extraction channel 302;
when the dosage of the solution to be measured needs to be changed, the installation position of the bolt 320 can be adjusted according to the accurate debugging scale on the rotating part 319, and the solution to be measured with the accurate quantitative proportion can be controlled.
Based on the above, the invention extracts a plurality of pulsatilla saponin components in the premix barrel 306 by arranging the injection barrel 1 on the frame 2 and arranging the sampling mechanism 3 and the liquid feed pump 5 at the side end of the material collecting frame 4, drives the rotating part 319 to rotate on the vortex tube 304 to and fro by the output end of the driving motor 301 through the vibration arm 315 and the rotating rod 316, determines that the solution is rapidly cooled to the solidification state at the upper part of the extraction channel 302 under the action of cold air in the vortex tube 303, and is vibrated to be in an uneven particle state by the continuous vibration and knock of the vibration arm 314 on the extraction channel 302, so that the vibration powder determination particles rapidly enter the lower part of the extraction channel 302 with a larger inclination angle through the opening and closing action of the stop valve 322, and can blow the remaining small amount of the determination solution attached to the lower part of the extraction channel 302 under the action of oblique hot air in the vortex tube 303, the measuring error caused by the loss of the measured solution dosage is avoided, and the measured solution with the required accurate quantitative proportion can be controlled by adjusting the installation position of the bolt 320 according to the accurate debugging scale on the rotating part 319;
the output shaft of the driving motor 301 drives the cam 305 to rotate, the flywheel 311 is driven to rotate by the first push rod 308 and the second push rod 310, the stirring fan 313 in the premixing cylinder 306 is driven to stir the internal mixed liquid so as to accelerate dissolution and rapidly separate out solid dosage preparation residues, and the preparation residues are screened by the filter plate 318, so that trace solid dosage preparation residues in the semisolid preparation are filtered, and frequent blockage of a chromatographic column in an HPLC instrument is avoided.
It will be appreciated by those skilled in the art that the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The embodiments disclosed above are therefore to be considered in all respects as illustrative and not restrictive. All changes which come within the scope of or equivalence to the invention are intended to be embraced therein.
Claims (8)
1. An analytical assay method for pharmaceutical use of a semisolid formulation based on HPLC, comprising the steps of:
s1: pretreatment for measurement: taking a proper amount of semisolid preparation medicine to be measured, putting the semisolid preparation medicine into the material injection cylinder body (1) and installing the semisolid preparation medicine on the rack (2);
s2: preparation of analytical measurement solution: dissolving the sample with methanol and acetonitrile single solvent or methanol-water, acetonitrile-water, methanol-acid and alkali, methanol-acid and acid ammonium salt water solution to extract multiple saponin components;
s3: the formulation residue was sieved and sampled accurately: screening residues of the solution by a sampling mechanism (3) arranged on the frame (2), filtering tiny solid residues, vibrating powder of the filtered solution at low temperature, sampling by accurate quantitative proportion, heating for a short time, flowing out the measured solution, and blowing off;
s4: chromatographic conditions are as follows: the chromatographic column is a reversed-phase chromatographic column, and the reversed-phase chromatographic column is selected from a phenyl silane bonded silica gel chromatographic column, an octadecyl silane bonded silica gel chromatographic column or an octaalkyl silane bonded silica gel chromatographic column;
taking a mixed solution of acid and alkali or acid and ammonium salt aqueous solution and an organic phase as a mobile phase, wherein the pH value of a water phase ranges from 2 to 8, and the organic phase is methanol or acetonitrile; performing gradient elution by adopting an isocratic or gradient elution method, wherein the volume ratio of the water phase in the mobile phase in isocratic elution is 90-60%, the ratio of the mobile phase in gradient elution is at time points of 0, 20-30, 32-35 and 36-45 min, and the volume ratio of the water phase is 80-75%, 20-30% and 20-80%;
s5: testing on a machine: and (4) injecting the analysis solution prepared in the step S3 into an HPLC instrument, performing chromatographic analysis, and recording a chromatogram.
2. An analytical method for pharmaceutical use of semi-solid preparations based on HPLC according to claim 1, characterized in that: the device is characterized in that a material collecting frame (4) is fixedly arranged at the upper end of the rack (2), and a liquid supply pump (5) communicated to the inside of the sampling mechanism (3) is installed at the side end of the material collecting frame (4).
3. An analytical method for pharmaceutical use of semi-solid preparations based on HPLC according to claim 2, characterized in that: the sampling mechanism (3) comprises a driving motor (301), an extraction channel (302) and a vortex tube (303), the driving motor (301) is installed on the rack (2) through an installation rack (304), a cam (305) is installed on an output shaft of the driving motor (301), a premixing barrel (306) is installed at the upper end of the material collecting rack (4), a supporting piece (307) is installed at the side end of the material collecting rack (4), a first push rod (308) is arranged on the supporting piece (307) in a sliding mode, a spring (309) is sleeved between the end portion, close to one side of the cam (305), of the first push rod (308) and the supporting piece (307), a second push rod (310) is hinged to the other end of the first push rod (308), a flywheel (311) is installed at the side end of the premixing barrel (306), the side end of the flywheel (311) is eccentrically hinged to the other end of the second push rod (310), and a stirring fan (313) is coaxially installed in the premixing barrel (306) and the flywheel (311), the other end of premixing section of thick bamboo (306) and stirring fan (313) coaxial arrangement have the arm (314) that shakes apart, the tip of driving motor (301) runs through support piece (307) and is connected with bull stick (315), the other end of bull stick (315) articulates there is bull stick two (316), the outer end of drawing passageway (302) is installed on frame (2) through mount (317), the upper end of drawing passageway (302) is passed through filter plate (318) and is linked through in the lower part of premixing section of thick bamboo (306), it is connected with rotation portion (319) to rotate on mounting bracket (304), the middle part of rotation portion (319) is articulated through adjustable bolt (320) and the other end of bull stick two (316), the tip of rotation portion (319) is provided with top (321), the middle part of drawing passageway (302) is provided with stop valve (322), vortex tube (303) are installed in the side of mounting bracket (304), one end of the vortex tube (303) is connected with the rotating part (319) through a first connecting tube (323), the other end of the vortex tube (303) is connected with a flow guide discharge tube (325) through a second connecting tube (324), and the other end of the flow guide discharge tube (325) is communicated with the lower side end of the extraction channel (302).
4. An analytical method for pharmaceutical use of semi-solid preparations based on HPLC according to claim 3, characterized in that: the inner bottom surface of the upper part of the extraction channel (302) is hinged with a plurality of uniformly distributed material blocking magnetic plates (326).
5. An analytical method for pharmaceutical use of semi-solid preparations based on HPLC according to claim 3, characterized in that: the rotating part (319) is of a hollow structure, and the end part connected with the top head (321) is matched with the side end surface of the extraction channel (302).
6. An analytical method for pharmaceutical use of semi-solid preparations based on HPLC according to claim 3, characterized in that: the whole extraction channel (302) is arranged in an inclined downward direction, and the lower inclined angle of the extraction channel (302) is relatively larger than the upper inclined angle of the extraction channel (302).
7. An analytical method for pharmaceutical use of semi-solid preparations based on HPLC according to claim 3, characterized in that: the flow guide discharge pipe (325) is obliquely arranged downwards relative to the lower part of the extraction channel (302).
8. An analytical method for pharmaceutical use of semi-solid preparations based on HPLC according to claim 3, characterized in that: the lower port of the extraction channel (302) is connected to an HPLC instrument.
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