CN204740205U - Device of sulfur dioxide volume of remaining in quick quantitative determination chinese -medicinal material - Google Patents
Device of sulfur dioxide volume of remaining in quick quantitative determination chinese -medicinal material Download PDFInfo
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- CN204740205U CN204740205U CN201520255771.5U CN201520255771U CN204740205U CN 204740205 U CN204740205 U CN 204740205U CN 201520255771 U CN201520255771 U CN 201520255771U CN 204740205 U CN204740205 U CN 204740205U
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Abstract
The utility model provides a device of sulfur dioxide volume of remaining in quick quantitative determination chinese -medicinal material, belongs to pharmaceutical analysis technical field. The device is including pure water bottle, sodium hydroxide solution bottle, two formalin bottles of adjacent benzene, ammonium acetate solution bottle, sodium hydrosulphite solution bottle, the little flow control type peristaltic pump of multichannel, reaction tank, ultrasonic instrument, little flow control type peristaltic pump, snakelike condenser pipe, filtration membrane, cell, detector, workstation. The device has instrument and easy operation, the testing result is accurate, can detect sulfur dioxide in the chinese -medicinal material effectively.
Description
Technical field
The utility model relates to the detection technique field of Sulphur Dioxide in Chinese Herbal Medicines by Iodine Titration Method, specifically a kind of device of mensuration of Sulphur Dioxide in Chinese Herbal Medicines by Iodine Titration Method, belongs to Pharmaceutical Analysis technical field.
Background technology
The sulfur dioxide residue of Chinese crude drug mainly exists with free state with in conjunction with the form of state, and free state comprises hydrosulfite (HSO
3 -), SO
2molecule and sulphite (SO
3 2-), and very easily formed various forms of in conjunction with state sulfur dioxide residue with reducing sugar, protein, pigment, enzyme, vitamin, aldehyde, ketone etc. in medicinal material.Because the sulphite of Irreversible binding does not dissociate under physiological environment, can not to health occurrence injury, therefore the detected object of general sulphuric dioxide or sulphite is free inferior sulfate radical and the sulphite of Reversible binding.
" Chinese Pharmacopoeia ", though version one in 2010 increases sulfur dioxide residual quantity determination method at annex, must be demarcated by arsenic trioxide before iodine titration solution uses, is unfavorable for the popularization of method; The method that bibliographical information measures Chinese crude drug sulfur dioxide residual quantity mainly contains hydrochloric para-rosaniline method, the chromatography of ions, high performance liquid chromatography and vapor-phase chromatography etc.Though above-mentioned detection method respectively has superiority, due to the difference of sample matrices, when detecting content of sulfur dioxide in different sample, need to adopt different detection methods, detection specificity, sensitivity still need to be further improved and enhanced.Angularly consider from technology raising, the export trade and guarantee people drug safety, set up the method for more advanced detection sulfur dioxide residual quantity in Chinese herbal medicine, on generaI investigation market, sulfur dioxide residue present situation the limitation proposing science are necessary greatly in Chinese crude drug.
Utility model content
Fundamental purpose of the present utility model is the deficiency overcoming above-mentioned prior art, set up the device of a kind of high specificity, highly sensitive alkalimetric titration-fluorescent spectrometry coupling mensuration sulfur dioxide residual quantity in Chinese herbal medicine, mainly solve the problems such as existing assay method measurement result is inaccurate.
In order to achieve the above object, the utility model provides a kind of method measuring sulfur dioxide residual quantity in Chinese herbal medicine, and the method comprises following processing step:
A. typical curve: drawing standard curve also releases computing formula.
In multiple reaction tank, add the sodium hydroxide solution of certain same volume and same concentrations respectively, then precision injects the sodium sulfite solution of finite concentration and certain gradient volume respectively, and precision injects ammonium acetate solution successively, and with after pure water dilution constant volume, stir lower slowly difference and slowly drip o-phthalaldehyde(OPA) solution successively, ultrasonic agitation 20min at 70 DEG C, be cooled to room temperature, add pure water constant volume; Be injected in 1cm cuvette after crossing film respectively, survey absorbance A in wavelength 354nm place, draw the typical curve of concentration and absorbance A, obtain regression equation.
B. sample determination: accurate weighing W mg Chinese crude drug is put into reaction tank, go to disperse Chinese crude drug with the sodium hydroxide solution of volume L1, the concentration of sodium hydroxide solution is identical with step a, and add ammonium acetate solution, after pure water dilution constant volume, stir lower slowly dropping o-phthalaldehyde(OPA) solution, the 365nm of uv analyzer is adopted to detect, until fluorescence color is constant, stop dripping o-phthalaldehyde(OPA) solution, at 70 DEG C, ultrasonic agitation 20min, 365nm detection fluorescence color is constant, add pure water constant volume, be cooled to room temperature; Inject 1cm cuvette after crossing film, survey absorbance A in wavelength 354nm place;
C. calculate content of sulfur dioxide in every kilogram of Chinese crude drug sample according to the typical curve of step a, the regression equation that the survey absorbance A obtained by step b brings step a into obtains the residual quantity of sulphuric dioxide.
Above-mentioned steps a is identical with the concentration of the sodium in NaOH after first time pure water dilution constant volume in b, and the mass ratio of second NaOH used and ammonium acetate is 15:0.76; In a with b, after second time NaOH pure water dilution constant volume, in NaOH, the concentration of sodium is identical.Step a is identical with the concentration of sodium hydroxide solution used in b, and the concentration of ammonium acetate solution is identical, and o-phthalaldehyde(OPA) solution concentration is identical.In step a, the consumption of o-phthalaldehyde(OPA) and the mass ratio of NaOH are 0.402:15.
Further preferably: a. typical curve: in multiple reaction tank, adds the sodium hydroxide solution that 3mL concentration is 5g/L respectively, then respectively accurate inject absorption 0.0,0.1,0.3,0.5,0.7,0.9,1.1,1.3, the 130mgL of 1.5mL
-1sodium sulfite solution, also distinguishes accurate injection 380mgL successively simultaneously
-1ammonium acetate solution 2mL, and after being diluted to 10mL with pure water, under stirring, slowly slowly drip 134mgL successively respectively
-1o-phthalaldehyde(OPA) solution 3mL, ultrasonic agitation 20min at 70 DEG C, is cooled to room temperature, adds pure water constant volume 25mL; Be injected in 1cm cuvette after crossing film respectively, survey absorbance A in wavelength 354nm place, drawing the typical curve (as seen accompanying drawing 1) of concentration and absorbance A, obtaining regression equation: A=87.03+517.32X, R
2=0.998.
B. sample determination: accurate weighing W mg Chinese crude drug is put into reaction tank, with the sodium hydroxide solution that volume L1, concentration are 5g/L go disperse Chinese crude drug, and add volume L2, concentration is 380mgL
-1ammonium acetate solution, after being diluted to volume L3, slowly drips 134mgL under stirring with pure water
-1o-phthalaldehyde(OPA) solution, adopts the 365nm of uv analyzer to detect, until fluorescence color is constant, stop dripping o-phthalaldehyde(OPA) solution, at 70 DEG C, ultrasonic agitation 20min, 365nm detection fluorescence color is constant, add pure water and be settled to volume L4, be cooled to room temperature; Inject 1cm cuvette after crossing film, survey absorbance A in wavelength 354nm place;
C. the typical curve according to step a calculates content of sulfur dioxide in every kilogram of Chinese crude drug sample:
In formula:
The content of sulphuric dioxide in Δ X-sample, mg/kg;
The strongest absorbance of A-mensuration sample liquid, L/ (gcm);
W-sample mass, mg.
In further preferred steps b, W mg:L1:L2:L3:L4 is 100mg:3mL:2mL:10mL:25mL.
Described Chinese crude drug was made into the dry medicinal material powder of 20 ~ 60 objects, directly carried out extraction and analysis detection; Solvent for use is water.Chinese crude drug is directly tested, and takes ultrasonic extraction.Directly fluorospectrophotometer test analysis is carried out after test drug solution is through removable filtering with microporous membrane.
Described Chinese crude drug to be measured is any one in lily, Poria cocos, safflower, the root of kudzu vine, reed rhizome, the tuber of dwarf lilyturf, asparagus fern, Radix Angelicae Sinensis, moutan bark, the root of herbaceous peony, the bark of eucommia, Radix Codonopsis, Chinese yam, fritillaria thunbergii, balloonflower root, Radix Isatidis, dried orange peel, coix seed, the Radix Astragali, the fruit of Chinese wolfberry, rhizoma atractylodis etc.
The device that the utility model adopts: a kind of device of fluorescence spectrum quantitative determination sulfur dioxide residual quantity, mainly comprise pure water bottle (1), sodium hydroxide solution bottle (2), o-phthalaldehyde(OPA) solution bottle (3), ammonium acetate solution bottle (4), sodium sulfite solution bottle (5), hyperchannel micrometeor control type peristaltic pump (6), reaction tank (7), Ultrasound Instrument (8), micrometeor control type peristaltic pump (9), serpentine condenser (10), filtering membrane (11), cuvette (12), detecting device (13), workstation (14).
Pure water bottle (1), sodium hydroxide solution bottle (2), o-phthalaldehyde(OPA) solution bottle (3), ammonium acetate solution bottle (4), sodium sulfite solution bottle (5) is connected with hyperchannel micrometeor control type peristaltic pump (6) respectively, and be communicated with reaction tank (7) by different passages, reaction tank (7) is placed in Ultrasound Instrument (8), reaction tank (7) is connected with filtering membrane (11) with serpentine condenser (10) by micrometeor control type peristaltic pump (9), filtering membrane (11) is connected with spectrophotometric cuvette (12), cuvette (12) is connected with detecting device (13), detecting device (13) is connected with workstation (14).
Pure water bottle (1), sodium hydroxide solution bottle (2), o-phthalaldehyde(OPA) solution bottle (3), ammonium acetate solution bottle (4), sodium sulfite solution bottle (5) are connected with hyperchannel micrometeor control type peristaltic pump (6) respectively, and this connects the silica gel hose adopting organic solvent-resistant and corrosion.Wherein, reaction tank (7) is glass material container, Ultrasound Instrument (8) should possess time controling, heating, agitating function simultaneously, serpentine condenser (10) is glass material container, filtering membrane (11) is removable miillpore filter, and cuvette (12) and detecting device (13) are placed in fluorospectrophotometer respectively.
The device of described fluorescent spectrometry quantitative determination sulfur dioxide residual quantity, wherein, the flow of the liquid of described reaction needed or volume are all controlled by hyperchannel micrometeor control type peristaltic pump or micrometeor control type peristaltic pump.
The device of described fluorescent spectrometry quantitative determination sulfur dioxide residual quantity, wherein, the temperature of reaction of reaction tank, stirring rate, reaction time control by Ultrasound Instrument.
The device of described fluorescent spectrometry quantitative determination sulfur dioxide residual quantity, wherein, reaction filtration unit is made up of peristaltic pump and miillpore filter, and wherein the aperture of miillpore filter is below 0.45 μm.
Hyperchannel micrometeor control type peristaltic pump is provided with between reservoir and reaction tank;
Ultrasonic reaction temperature, mixing time are controlled by Ultrasound Instrument;
In reservoir, liquid suction tube head is installed the filtrator of anti-suck.
Compared with the prior art the assay method of Sulphur Dioxide in Chinese Herbal Medicines by Iodine Titration Method described in the utility model has outstanding substantive distinguishing features and marked improvement, 1. concentration is adopted to be that the sodium hydroxide solution of 5g/L absorbs and the sulphite of the free state dissolved in Chinese crude drug and reversible state, there is good dispersion effect and effectively prevent the volatilization loss of sulphuric dioxide, make measurement result closer to actual numerical value; 2. this law is 6.6 × 10 to the minimum detectability of sulphuric dioxide
-3mg/Kg Chinese crude drug; 3. this law is about 30min detection time.Therefore, method of the present utility model is sensitive, accurate, easy, is applicable to detect various Sulphur Dioxide in Chinese Herbal Medicines by Iodine Titration Method is residual.The device of described fluorescent spectrometry quantitative determination sulfur dioxide residual quantity, compared with prior art, has structure simple, easy to operate, not by artificial interference; This device not only can automatic liquid-feeding, and liquid volume added controls precisely, to improve detection efficiency.
Accompanying drawing explanation
Fig. 1 is content of sulfur dioxide typical curve.
Fig. 2 is alkalimetric titration-fluorescence spectrum combined apparatus schematic diagram used in method of the present utility model.In figure, 1 pure water bottle, 2 sodium hydroxide solution bottles, 3 o-phthalaldehyde(OPA) solution bottles, 4 ammonium acetate solution bottles, 5 sodium sulfite solution bottles, 6 hyperchannel micrometeor control type peristaltic pumps, 7 reaction units, 8 Ultrasound Instrument, 9 micrometeor control type peristaltic pumps, 10 cooling devices, 11 filtration units, 12 cuvettes, 13 detecting devices, 14 workstations, 15 reaction units, 16 filtration units, 17 fluorospectrophotometers.
Embodiment
Below in conjunction with embodiment, the utility model is described further, but the utility model is not limited to following examples.
Accompanying drawing 2 is shown in by concrete proving installation.
A kind of device of fluorescent spectrometry quantitative determination sulfur dioxide residual quantity, mainly comprise pure water bottle 1, sodium hydroxide solution bottle 2, o-phthalaldehyde(OPA) solution bottle 3, ammonium acetate solution bottle 4, sodium sulfite solution bottle 5, hyperchannel micrometeor control type peristaltic pump 6, reaction tank 7, Ultrasound Instrument 8, micrometeor control type peristaltic pump 9, serpentine condenser 10, filtering membrane 11, cuvette 12, detecting device 13, workstation 14, above-mentioned part needs the silica gel hose of employing organic solvent-resistant and the corrosion connected.Wherein, reaction tank 7 is glass material container, and Ultrasound Instrument 8 should possess time controling, heating, agitating function simultaneously, and serpentine condenser 10 is glass material container, filtering membrane 11 is removable miillpore filter, and cuvette 12 and detecting device 13 are placed in fluorospectrophotometer respectively.
The device of fluorescent spectrometry quantitative determination sulfur dioxide residual quantity described in the present embodiment, wherein, describedly respectively a certain amount of sodium hydroxide solution bottle 2, o-phthalaldehyde(OPA) solution bottle 3, ammonium acetate solution bottle 4 are injected reaction tank 7 by hyperchannel micrometeor control type peristaltic pump 6, then draw a certain amount of water constant volume from pure water bottle 1.Described Ultrasound Instrument 8 can control reaction stirring rate, temperature of reaction, reaction time.In the solution of described reaction tank 7 injects fluorospectrophotometer cuvette by micrometeor control type peristaltic pump 9, serpentine condenser 10 and filtering membrane 11 12, enter spectrophotometric analysis by detecting device 13, show result at workstation 14.Hyperchannel micrometeor control type peristaltic pump 6 is opened after detection terminates, extract the pure water washing pipe road in pure water bottle 1, drain waste liquid, after waste liquid is drained, closes all switches, and cleaning reaction device and cuvette, now complete an automatic testing process of sulfur dioxide residual quantity.
Embodiment 1
Measure the content of sulphuric dioxide in asparagus fern, step is:
A. typical curve: in reaction tank, adds the sodium hydroxide solution that 3mL concentration is 5g/L respectively, then respectively accurate inject absorption 0.0,0.1,0.3,0.5,0.7,0.9,1.1,1.3, the 130mgL of 1.5mL
-1sodium sulfite solution, also distinguishes accurate injection 380mgL successively simultaneously
-1ammonium acetate solution 2mL, and after being diluted to 10mL with pure water, under stirring, slowly slowly drip 134mgL successively respectively
-1o-phthalaldehyde(OPA) solution 3mL, ultrasonic agitation 20min at 70 DEG C, is cooled to room temperature, adds pure water constant volume 25mL; Be injected in 1cm cuvette after crossing film respectively, survey absorbance A in wavelength 354nm place, drawing the typical curve (as seen accompanying drawing 1) of concentration and absorbance A, obtaining regression equation: A=87.03+517.32X, R
2=0.998.
B. sample determination: accurate weighing 100mg Chinese crude drug asparagus fern is put into 50mL reaction tank, go to disperse Chinese crude drug, and to add 2mL concentration is 380mgL with the sodium hydroxide solution that 3mL concentration is 5g/L
-1ammonium acetate solution, after being diluted to 10mL, slowly drips 134mgL under stirring with pure water
-1o-phthalaldehyde(OPA) solution, adopts the 365nm of uv analyzer to detect, until fluorescence color is constant, stops dripping o-phthalaldehyde(OPA) solution, and at 70 DEG C, ultrasonic agitation 20min, 365nm detection fluorescence color is constant, adds pure water and is settled to 25mL, be cooled to room temperature; Inject 1cm cuvette after crossing film, survey absorbance 155.008 in wavelength 354nm place;
C. the typical curve according to step a calculates content of sulfur dioxide in every kilogram of Chinese crude drug asparagus fern:
In formula:
The content of sulphuric dioxide in Δ X-sample, mg/kg;
The strongest absorbance of A-mensuration sample liquid, L/ (gcm);
M-sample mass, mg.
Replicate determination five times, the results are shown in Table 1;
Embodiment 2
Measure the content of sulphuric dioxide in fritillaria thunbergii, step is:
Accurate weighing 100mg is pulverized uniform commercially available fritillaria thunbergii sample, and sample preparation and other operations are with embodiment 1, and sample is crossed film and injected 1cm cuvette, and surveying absorbance in wavelength 354nm place is 308.315.
The content of sulphuric dioxide in calculation sample:
Replicate determination five times, the results are shown in Table 1;
Embodiment 3
Measure the content of sulphuric dioxide in Poria cocos, step is:
Accurate weighing 50mg is pulverized uniform commercially available Poria cocos sample, and sample preparation and other operations are with embodiment 1, and sample is crossed film and injected 1cm cuvette, and surveying absorbance in wavelength 354nm place is 262.846.
The content of sulphuric dioxide in calculation sample:
Replicate determination five times, the results are shown in Table 1;
Embodiment 4
Measure the content of sulphuric dioxide in Radix Isatidis, step is:
Accurate weighing 100mg is pulverized uniform commercially available Radix Isatidis sample, and sample preparation and other operations are with embodiment 1, and sample is crossed film and injected 1cm cuvette, and surveying absorbance in wavelength 354nm place is 93.184.
The content of sulphuric dioxide in calculation sample:
Replicate determination five times, the results are shown in Table 1;
Table 1 the utility model embodiment compares with CP method (distillation titrimetry) measurement result.
Due to " Chinese Pharmacopoeia " though version one in 2010 adopts sour distilled-iodimetry in the method for annex detection sulfur dioxide residual quantity, this method first by sample in closed container with after HCl treatment, distill and pass into the sulphuric dioxide that nitrogen blows out release, absorb through hydrogen peroxide oxidation, add methyl red indicator, use sodium hydroxide solution titration, the sodium hydroxide solution of actual consumption converts its sulfur dioxide residual quantity per sample; This method approximately needs 2 ~ 3h from mounting glass distillation and absorption plant to detection of end, consuming time longer, larger by man's activity in operating process.
Above-described embodiment is only for the utility model example is clearly described, and is not to restriction of the present utility model.For the routine experimentation personnel in affiliated field, can also make other changes in different forms on the basis of the above description.All do within spirit of the present utility model and principle any amendment, equivalent to replace and improvement etc., all belong within scope of the present utility model.
Claims (4)
1. the device of a quantitative determination sulfur dioxide residual quantity in Chinese herbal medicine, it is characterized in that, mainly comprise pure water bottle (1), sodium hydroxide solution bottle (2), o-phthalaldehyde(OPA) solution bottle (3), ammonium acetate solution bottle (4), sodium sulfite solution bottle (5), hyperchannel micrometeor control type peristaltic pump 888 (6), reaction tank (7), Ultrasound Instrument (8), micrometeor control type peristaltic pump (9), serpentine condenser (10), filtering membrane (11), cuvette (12), detecting device (13), workstation (14),
Pure water bottle (1), sodium hydroxide solution bottle (2), o-phthalaldehyde(OPA) solution bottle (3), ammonium acetate solution bottle (4), sodium sulfite solution bottle (5) is connected with hyperchannel micrometeor control type peristaltic pump (6) respectively, and be communicated with reaction tank (7) by different passages, reaction tank (7) is placed in Ultrasound Instrument (8), reaction tank (7) is connected with filtering membrane (11) with serpentine condenser (10) by micrometeor control type peristaltic pump (9), filtering membrane (11) is connected with spectrophotometric cuvette (12), cuvette (12) is connected with detecting device (13), detecting device (13) is connected with workstation (14).
2. according to the device of a kind of quantitative determination sulfur dioxide residual quantity in Chinese herbal medicine according to claim 1, it is characterized in that, pure water bottle (1), sodium hydroxide solution bottle (2), o-phthalaldehyde(OPA) solution bottle (3), ammonium acetate solution bottle (4), sodium sulfite solution bottle (5) are connected with hyperchannel micrometeor control type peristaltic pump (6) respectively, and this connects the silica gel hose adopting organic solvent-resistant and corrosion; Reaction tank (7) is glass material container, Ultrasound Instrument (8) should possess time controling, heating, agitating function simultaneously, serpentine condenser (10) is glass material container, filtering membrane (11) is removable miillpore filter, and cuvette (12) and detecting device (13) are placed in fluorospectrophotometer respectively.
3. according to the device of a kind of quantitative determination sulfur dioxide residual quantity in Chinese herbal medicine according to claim 1, it is characterized in that, filtering membrane (11) is miillpore filter, and wherein the aperture of miillpore filter is below 0.45 μm.
4. according to the device of a kind of quantitative determination sulfur dioxide residual quantity in Chinese herbal medicine according to claim 1, it is characterized in that, between reservoir and reaction tank, be provided with hyperchannel micrometeor control type peristaltic pump;
Ultrasonic reaction temperature, mixing time are controlled by Ultrasound Instrument;
In reservoir, liquid suction tube head is installed the filtrator of anti-suck.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104977266A (en) * | 2015-04-24 | 2015-10-14 | 河北中医学院 | Apparatus and method for rapidly measuring sulfur dioxide residue level in Chinese herb |
| CN115356180A (en) * | 2022-10-24 | 2022-11-18 | 莱阳市检验检测中心 | Food safety detector |
-
2015
- 2015-04-24 CN CN201520255771.5U patent/CN204740205U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104977266A (en) * | 2015-04-24 | 2015-10-14 | 河北中医学院 | Apparatus and method for rapidly measuring sulfur dioxide residue level in Chinese herb |
| CN104977266B (en) * | 2015-04-24 | 2017-08-04 | 河北中医学院 | A kind of device and method of quantitative determination sulfur dioxide residual quantity in Chinese herbal medicine |
| CN115356180A (en) * | 2022-10-24 | 2022-11-18 | 莱阳市检验检测中心 | Food safety detector |
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