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CN108802224A - A kind of high-precision traditional Chinese medicine ingredients liquid chromatography system - Google Patents

A kind of high-precision traditional Chinese medicine ingredients liquid chromatography system Download PDF

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Publication number
CN108802224A
CN108802224A CN201810615830.3A CN201810615830A CN108802224A CN 108802224 A CN108802224 A CN 108802224A CN 201810615830 A CN201810615830 A CN 201810615830A CN 108802224 A CN108802224 A CN 108802224A
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chinese medicine
traditional chinese
medicine ingredients
liquid chromatography
detection device
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CN201810615830.3A
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CN108802224B (en
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贾洪斌
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Xiao Fei
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Weifang University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N2030/022Column chromatography characterised by the kind of separation mechanism
    • G01N2030/027Liquid chromatography

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

The invention discloses a kind of high-precision traditional Chinese medicine ingredients liquid chromatography systems, include mainly infusion device, sample processing device, liquid-phase chromatographic column, detection device, control device, data analysis set-up and collection device, infusion device is located at the upper left side of analytical equipment, including mobile phase storage tank, filter, high-pressure pump, degasser and relief valve;Sample processing device is arranged on the right side of infusion device, including feed inlet, grinding device, strainer valve, dilution extraction element, injector and reversal valve;The right lateral surface in analytical equipment is arranged in liquid-phase chromatographic column;Detection device is arranged in the lower section of sample processing device, including sample stage, X-ray source, first collimator, analyzing crystal, the second collimator and detector;Control device is arranged in the left side of detection device.In short, the present invention has many advantages, such as that structure novel, high degree of automation, testing result are accurate.

Description

A kind of high-precision traditional Chinese medicine ingredients liquid chromatography system
Technical field
The invention belongs to drug ingedient analysis technical fields, are specifically related to a kind of high-precision traditional Chinese medicine ingredients liquid chromatogram point Analysis apparatus.
Background technology
Chinese medicine is the precious legacy in China, as Chinese medicine is at home and abroad applied increasingly extensive, how to solve herbal species Particularly important, many Chinese medicines of the problems such as confusion, quality decline, influence Chinese Herbs, the adulterant of especially valuable short medicinal material It is found more, seriously affects clinical efficacy and export abroad or even threat to life safety sometimes, and forge technology increasingly Height, only according to general traditional discrimination method be difficult to it is accurate, rapidly differentiate them.Therefore, it finds accurately and reliably, it is easy to be easy Row, the advanced TCD identificafion method of system, oneself is paid attention to by people, traditional detect by an unaided eye medicinal material section, powder or extraction The fluorescence of object differentiates the method for the Chinese medicine true and false, though having longer history, because its subjective error is larger, lacks standard drawing The reasons such as the control of spectrum, and greatly limit its application and development.
Liquid chromatogram abbreviation HPLC, also known as high speed or high pressure liquid chromatography.The method absorbs common liquid chromatography and gas phase The advantages of chromatography, grows up by being suitably modified, the function of existing common liquid chromatography, and has the characteristics of gas-chromatography (i.e. high pressure, high speed, high-resolution and high sensitivity).HPLC is the novel isolation technics developed rapidly in recent years, Be applicable not only to it is many not volatile, hardly possible thermal decomposition substance (such as protein, peptides, amino acid and its derivative etc.) it is qualitative fixed Amount analysis, and it is also applied for the preparation and separation of above-mentioned substance.HPLC methods are due to having both two kinds of chromatography of liquid and gas The advantages of method, is applied and develops rapidly in food inspection and analysis in recent years.Liquid chromatogram (HPLC) is to combine classical liquid The separation principle of phase chromatography and gas-chromatography.Since compared with gas chromatography, liquid chromatography has following major advantage:① The not limitation of the volatility of test sample and thermal stability, has a wide range of application;2. various solvents of different nature can be selected as stream Dynamic phase, and the selectivity for flowing relative separation has great role, therefore separation selectivity is high;3. generally at ambient temperature into Row separation, does not need high column temperature.Thus it is widely used in biochemistry, biomedical, petrochemical industry, synthesis chemistry, environment prison It surveys, food hygiene and commodity inspection, many analytical control departments such as method inspection and quality inspection.
Liquid chromatograph is a kind of strong analysis tool, so design is a kind of to carry out traditional Chinese medicine ingredients point using liquid chromatogram Analysis apparatus very it is necessary to.
Invention content
For the above-mentioned prior art the problem of, the present invention provides a kind of high-precision traditional Chinese medicine ingredients liquid chromatograies point Analysis apparatus.
The technical scheme is that:A kind of high-precision traditional Chinese medicine ingredients liquid chromatography system, main includes infusion dress It sets, sample processing device, liquid-phase chromatographic column, detection device, control device, data analysis set-up and collection device, the infusion Device is located at the upper left side of analytical equipment, and infusion device includes mobile phase storage tank, filter, high-pressure pump, degasser and lets out Pressure valve, the mobile phase storage tank are arranged in the top of infusion device, and the filter is mounted on the left-hand face of infusion device, The inside left in infusion device is arranged in the high-pressure pump, and the degasser is arranged in the right side of high-pressure pump, the relief valve Mounted on the lower section of degasser, mobile phase storage tank, filter, high-pressure pump and degasser pass sequentially through pipeline and connect;Institute It states sample processing device to be arranged on the right side of infusion device, sample processing device includes feed inlet, grinding device, strainer valve, dilute Extraction element, injector and reversal valve are released, the feed inlet is arranged in the top of sample processing device, and is stored positioned at mobile phase The right side of tank, the grinding device are arranged in the lower section of feed inlet, and the dilution extraction element is connected to by the strainer valve The lower section of grinding device, dilution extraction element inner right side are equipped with ultrasonic extraction device, and the injector is mounted on grinding device Right side, and positioned at the top of ultrasonic extraction device, the reversal valve is arranged on the right side of ultrasonic extraction device;The liquid phase color The right lateral surface in analytical equipment is arranged in spectrum column;The detection device is arranged in the lower section of sample processing device, detection device packet Sample stage, X-ray source, first collimator, analyzing crystal, the second collimator and detector are included, the sample stage is mounted on inspection The lower right corner of device is surveyed, the X-ray source is arranged on the right side inner wall of detection device, and X-ray source is towards sample stage, The first collimator is arranged in the top of sample stage, and the analyzing crystal is mounted on the inner tip of detection device, and described the Two collimators are arranged in the left side of first collimator, and the detector is mounted on the lower left corner of detection device;The control device It is arranged in the left side of detection device;The data analysis set-up is arranged in the lower section of control device, and data analysis set-up and institute State detector electric connection;The collection device is arranged in the lower section of detection device.
Further, the liquid-phase chromatographic column includes into Xiang Kou, cylinder, filler, temperature control box and photo outlet, the cylinder Be arranged inside the temperature control box, described to be arranged into phase mouth in the upper end of cylinder, the filler is located at column body, it is described go out Phase mouth is arranged in the lower end of cylinder, and liquid-phase chromatographic column can detach the heterogeneity in Chinese medicine, convenient for traditional Chinese medicine ingredients Analysis.
Further, the control device includes display screen, control button, controller and printing equipment, the display screen Front surface in control device is set, and the control button is arranged on the right side of display screen, and the controller setting is filled in control The inside set, the printing equipment are mounted on the lower section of display screen and control button, and control device can be set with personnel easy to operation Set device parameter and artificial manipulation.
Further, temperature controller is equipped in the temperature control box, the temperature controller is electrically connected with controller, and temperature controller can be with Adjust the temperature in temperature control box so that liquid-phase chromatographic column operating ambient temperature reaches optimum temperature, and operating personnel can pass through control Device processed adjusts the temperature in temperature control box.
Further, cycle has been passed through cooling water inside the X-ray source, and X-ray source is when emitting X-ray, only It can say that 0.2% or so power consumption is converted to X-ray, remaining power consumption is changed into thermal energy, and cycle is logical as cooling water avoids X-ray light Source temperature is excessively high to be damaged.
Further, the dilution extraction element rear surface is equipped with pure water tank and drain valve, and the drain valve is located at pure water The lower section of case, pure water tank are used for being diluted with water herb powder in dilution extraction element, and drain valve is clear for sample processing device The discharge of wash water.
Further, analytical equipment rear surface lower part is equipped with radiator and power cord, and detection device and analysis fill It sets and will produce amount of heat at work, radiator can avoid high temperature from damaging device quickly by heat derives.
The present invention operation principle be:A kind of high-precision traditional Chinese medicine ingredients liquid chromatography system provided by the invention, into When row traditional Chinese medicine ingredients are analyzed, first Chinese medicine is added to through feed inlet in grinding device, enters dilution through strainer valve after crushing Extraction element, pure water tank add water to dilution extraction element, active ingredient extraction are carried out through ultrasonic extraction device after dilution, after standing Injector takes supernatant to input reversal valve, and the mobile phase in mobile phase storage tank is pumped by high-pressure pump through filter and degasser Reversal valve is brought traditional Chinese medicine sample into liquid-phase chromatographic column, is detached to traditional Chinese medicine ingredients, and the sample after separation enters in detection device Sample stage, X-ray source irradiating sample generates fluorescent x ray, and fluorescent x ray forms parallel light beam through first collimator and penetrate To analyzing crystal, analyzing crystal separates the fluorescent x ray of different wave length, and then entering detector through the second collimator is examined It surveys, detection data is transmitted to data analysis set-up by detector, and analysis result is printed through printing equipment after analysis completion.
The beneficial effects of the invention are as follows:A kind of high-precision traditional Chinese medicine ingredients liquid chromatography system provided by the invention, especially It is suitable for the analyses of various traditional Chinese medicine ingredients, stand crushing Chinese medicine plus after water stirring and are carried by way of taking supernatant Chinese medicine sample is taken, high temperature extraction is avoided or centrifugation extraction is damaged or influenced on traditional Chinese medicine ingredients, infusion device is equipped with pressure release Valve, blocks convenient for infusion device and excludes overpressure, and detection device selects X-ray fluorescence spectra analytical equipment, x-ray fluorescence light Spectrum analysis device performance is stablized, and detection sensitivity is high, and the data after detection have printing to fill after data molecular device separating treatment Printing testing result is set, whole increasingly automated, the present apparatus is additionally provided with control device, and operating personnel can manually control each link Detection parameters.In short, the present invention has many advantages, such as that structure novel, high degree of automation, testing result are accurate.
Description of the drawings
Fig. 1 is the overall structure diagram of the present invention;
Fig. 2 is the rearview of the present invention.
Wherein, 1- infusion devices, 101- mobile phases storage tank, 102- filters, 103- high-pressure pumps, 104- degassers, 105- relief valves, 2- sample processing devices, 201- feed inlets, 202- grinding devices, 203- strainer valves, 204- dilution extraction dresses Set, 205- injectors, 206- reversal valves, 207- pure water tanks, 208- drain valves, 209- ultrasonic extraction devices, 3- liquid-phase chromatographic columns, 301- into Xiang Kou, 302- cylinder, 303- fillers, 304- temperature control boxs, 3041- temperature controllers, 305- photo outlets, 4- detection devices, 401- sample stages, 402-X ray sources, 403- first collimators, 404- analyzing crystals, the second collimators of 405-, 406- detections Device, 5- control devices, 501- display screens, 502- control buttons, 503- printing equipments, 6- data analysis set-ups, 7- collection devices, 8- radiators, 9- power cords.
Specific implementation mode
For ease of the understanding to technical solution of the present invention, below in conjunction with the accompanying drawings 1-2 and specific embodiment to the present invention do into The explanation of one step, embodiment do not constitute the restriction to invention protection domain.
Include mainly infusion device 1, at sample as shown in Figure 1, a kind of high-precision traditional Chinese medicine ingredients liquid chromatography system Manage device 2, liquid-phase chromatographic column 3, detection device 4, control device 5, data analysis set-up 6 and collection device 7, infusion device 1 In the upper left side of analytical equipment, infusion device 1 includes mobile phase storage tank 101, filter 102, high-pressure pump 103, degasser 104 and relief valve 105, mobile phase storage tank 101 is arranged in the top of infusion device 1, and filter 102 is mounted on infusion device 1 Left-hand face, the inside left in infusion device 1 is arranged in high-pressure pump 103, and degasser 104 is arranged on the right side of high-pressure pump 103 Side, relief valve 105 are mounted on the lower section of degasser 104, mobile phase storage tank 101, filter 102, high-pressure pump 103 and degassing Device 104 passes sequentially through pipeline connection;Sample processing device 2 is arranged on the right side of infusion device 1, and sample processing device 2 includes Feed inlet 201, grinding device 202, strainer valve 203, dilution extraction element 204, injector 205 and reversal valve 206, feed inlet 201 are arranged in the top of sample processing device 2, and positioned at mobile phase storage tank 101 right side, grinding device 202 setting into The lower section of material mouth 201, dilution extraction element 204 are connected to the lower section of grinding device 202, dilution extraction dress by strainer valve 203 It sets 204 inner right sides and is equipped with ultrasonic extraction device 209, injector 205 is mounted on the right side of grinding device 202, and positioned at ultrasound The top of extraction element 209, reversal valve 206 are arranged on the right side of ultrasonic extraction device 209, dilute 204 rear surface of extraction element Equipped with pure water tank 207 and drain valve 208, drain valve 208 is located at the lower section of pure water tank 207;The setting of liquid-phase chromatographic column 3 is filled in analysis The right lateral surface set, liquid-phase chromatographic column 3 include into phase mouth 301, cylinder 302, filler 303, temperature control box 304 and photo outlet 305, Cylinder 302 is arranged inside temperature control box 304, and temperature controller 3041, temperature controller 3041 and 503 electricity of controller are equipped in temperature control box 304 Property connection, be arranged into phase mouth 301 in the upper end of cylinder 302, filler 303 is located inside cylinder 302, photo outlet 305 be arranged exists The lower end of cylinder 302;Detection device 4 is arranged in the lower section of sample processing device 2, and detection device 4 includes sample stage 401, X-ray Light source 402, first collimator 403, analyzing crystal 404, the second collimator 405 and detector 406, sample stage 401 are mounted on inspection The lower right corner of device 4 is surveyed, X-ray source 402 is arranged on the right side inner wall of detection device 4, and X-ray source 402 is towards sample Sample platform 401, X-ray source inside cycle have been passed through cooling water, and first collimator 404 is arranged in the top of sample stage 401, light splitting Crystal 404 is mounted on the inner tip of detection device 4, and the second collimator 405 is arranged in the left side of first collimator 403, detection Device 406 is mounted on the lower left corner of detection device 4;Control device 5 is arranged in the left side of detection device 4, and control device 5 includes display The front surface in control device 5 is arranged in screen 501, control button 502, controller and printing equipment 503, display screen 501, and control is pressed Key 502 is arranged on the right side of display screen 501, and controller is arranged in the inside of control device 5, and printing equipment 503 is mounted on display The lower section of screen 501 and control button 502;Data analysis set-up 6 is arranged in the lower section of control device 5, and data analysis set-up 6 with Detector 406 is electrically connected;Collection device 7 is arranged in the lower section of detection device 4, as shown in Fig. 2, analytical equipment rear surface lower part Equipped with radiator 8 and power cord 9.
The working method of the present embodiment is:When carrying out traditional Chinese medicine ingredients analysis, first Chinese medicine is added to through feed inlet 201 In grinding device 202, enter dilution extraction element 204 through strainer valve 203 after crushing, pure water tank 207 adds water to dilution extraction dress 204 are set, active ingredient extraction is carried out through ultrasonic extraction device 209 after dilution, injector 205 takes supernatant input commutation after standing Mobile phase in mobile phase storage tank 101 is pumped into reversal valve by valve 206, high-pressure pump 103 through filter 102 and degasser 104 206, it brings traditional Chinese medicine sample into liquid-phase chromatographic column 3, traditional Chinese medicine ingredients is detached, the sample after separation enters in detection device 4 Sample stage 401,402 irradiating sample of X-ray source, generate fluorescent x ray, fluorescent x ray forms parallel through first collimator 403 Light beam directive analyzing crystal 404, analyzing crystal 404 separates the fluorescent x ray of different wave length, then through the second collimator 405 It is detected into detector 406, detection data is transmitted to data analysis set-up 6 by detector 406, through printing after analysis completion Device 503 prints analysis result.
Finally it should be noted that:The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations;Although Present invention has been described in detail with reference to the aforementioned embodiments, it will be understood by those of ordinary skill in the art that:It still may be used To modify to the technical solution recorded in previous embodiment or equivalent replacement of some of the technical features;And These modifications or replacements, the spirit and model of technical solution of the embodiment of the present invention that it does not separate the essence of the corresponding technical solution It encloses.

Claims (7)

1. a kind of high-precision traditional Chinese medicine ingredients liquid chromatography system, which is characterized in that include mainly infusion device (1), sample Processing unit (2), liquid-phase chromatographic column (3), detection device (4), control device (5), data analysis set-up (6) and collection device (7), the infusion device (1) is located at the upper left side of analytical equipment, and infusion device (1) includes mobile phase storage tank (101), filtering Device (102), high-pressure pump (103), degasser (104) and relief valve (105), the mobile phase storage tank (101) are arranged defeated The top of liquid device (1), the filter (102) are mounted on the left-hand face of infusion device (1), and the high-pressure pump (103) sets The inside left in infusion device (1) is set, the degasser (104) is arranged in the right side of high-pressure pump (103), the relief valve (105) be mounted on degasser (104) lower section, mobile phase storage tank (101), filter (102), high-pressure pump (103) and take off Device of air (104) passes sequentially through pipeline connection;The sample processing device (2) is arranged at the right side of infusion device (1), sample Reason device (2) includes feed inlet (201), grinding device (202), strainer valve (203), dilution extraction element (204), injector (205) it is deposited in the top of sample processing device (2), and positioned at mobile phase with reversal valve (206), feed inlet (201) setting The right side of storage tank (101), the grinding device (202) are arranged in the lower section of feed inlet (201), the dilution extraction element (204) lower section of grinding device (202) is connected to by the strainer valve (203), dilution extraction element (204) inner right side is set There is ultrasonic extraction device (209), the injector (205) is mounted on the right side of grinding device (202), and is filled positioned at ultrasonic extraction Set the top of (209), right side of reversal valve (206) setting in ultrasonic extraction device (209);The liquid-phase chromatographic column (3) Right lateral surface in analytical equipment is set;The detection device (4) is arranged in the lower section of sample processing device (2), detection device (4) include sample stage (401), X-ray source (402), first collimator (403), analyzing crystal (404), the second collimator (405) and detector (406), the sample stage (401) are mounted on the lower right corner of detection device (4), the X-ray source (402) it is arranged on the right side inner wall of detection device (4), and X-ray source (402) is accurate towards sample stage (401), described first In the top of sample stage (401), the inside that the analyzing crystal (404) is mounted on detection device (4) is pushed up for straight device (404) setting End, in the left side of first collimator (403), the detector (406) is mounted on detection and fills for the second collimator (405) setting Set the lower left corner of (4);Left side of control device (5) setting in detection device (4);Data analysis set-up (6) setting Lower section in control device (5), and data analysis set-up (6) is electrically connected with the detector (406);The collection device (7) lower section of the setting in detection device (4).
2. a kind of high-precision traditional Chinese medicine ingredients liquid chromatography system according to claim 1, which is characterized in that the liquid Phase chromatographic column (3) includes into Xiang Kou (301), cylinder (302), filler (303), temperature control box (304) and photo outlet (305), institute It is internal in the temperature control box (304) to state cylinder (302) setting, it is described to be arranged into Xiang Kou (301) in the upper end of cylinder (302), institute It states filler (303) and is located at cylinder (302) inside, lower end of photo outlet (305) setting in cylinder (302).
3. a kind of high-precision traditional Chinese medicine ingredients liquid chromatography system according to claim 1, which is characterized in that the control Device (5) processed includes display screen (501), control button (502), controller and printing equipment (503), the display screen (501) Front surface in control device (5) is set, and the control button (502) is arranged in the right side of display screen (501), the controller Inside in control device (5) is set, and the printing equipment (503) is mounted under display screen (501) and control button (502) Side.
4. a kind of high-precision traditional Chinese medicine ingredients liquid chromatography system according to claim 1, which is characterized in that the temperature It controls and is equipped with temperature controller (3041) in case (304), the temperature controller (3041) is electrically connected with controller (503).
5. a kind of high-precision traditional Chinese medicine ingredients liquid chromatography system according to claim 1, which is characterized in that described dilute It releases extraction element (204) rear surface and is equipped with pure water tank (207) and drain valve (208), the drain valve (208) is located at pure water tank (207) lower section.
6. a kind of high-precision traditional Chinese medicine ingredients liquid chromatography system according to claim 1, which is characterized in that described point Analysis apparatus rear surface lower part is equipped with radiator (8) and power cord (9).
7. a kind of high-precision traditional Chinese medicine ingredients liquid chromatography system according to claim 1, which is characterized in that described dilute It releases extraction element (204) rear surface and is equipped with drain valve (208).
CN201810615830.3A 2018-06-14 2018-06-14 High accuracy traditional chinese medicine composition liquid chromatography analytical equipment Expired - Fee Related CN108802224B (en)

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