CN102590416A - Method for extracting negative ions from extract medicine by means of matrix solid phase dispersion and ion chromatographic detection method - Google Patents
Method for extracting negative ions from extract medicine by means of matrix solid phase dispersion and ion chromatographic detection method Download PDFInfo
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Abstract
The invention relates to a method for extracting negative ions from an extract medicine by means of matrix solid phase dispersion and an ion chromatographic detection method. A raw material of a vegetable medicine and solid phase extracting agents (namely graphitized carbon and SPE (solid phase extraction) C18) are uniformly grinded together, are subjected to solid phase extraction and then are eluted by deionized water, finally the eluted solution is an extracting solution containing negative ions. The eluted solution is diluted by the deionized water to be at the required concentration, then the solution is extracted to be filtered by a filter film of 0.22um, and the filtered solution is a solution to be detected. The filtered solution is tested by an ion chromatographic analyzer, the tested seven kinds of inorganic negative ions, namely F<->, Cl<->, NO2<->, Br<->, NO3<->, PO4<3-> and SO4<2->, have excellent linear relations within the range of 0.4-12mg/L, the detection limit is 1.20-5.00ug/L, the recovery is 70%-98%, and the degree of precision is 2.09%-5.87%.
Description
One, technical field
The present invention relates to a kind of matrix solid phase and disperse to extract negative ion and chromatography of ions detection method in the medicine, belong to chemical extraction and chromatography of ions detection technique field.
Two, background technology
Matrix solid phase dispersion technology (MSPD, matrix solid-phase dispersion) is the Barker professor of U.S. Louisiana state university proposed and gave theoretical explanation in 1989 a kind of quick sample treatment technology.Its advantage is to have concentrated processes such as sample homogenize in traditional sample pre-treatments, histocyte cracking, extraction, purification, need not carry out operation stepss such as tissue homogenate, deposition, centrifugal, pH regulator and sample transfer, has avoided the loss of sample.It is a kind of extraction and cleaning method of simple highly effective, is applicable to the extraction and cleaning of various molecular structures and polarity residues of pesticides, has improved analysis speed, has reduced reagent dosage, has been suitable for automated analysis.
China's autonomic drug development at present is in period in the ascendant, and therefore wherein the qualitative and quantitative analysis of chemical constitution seems of crucial importance in the autonomic drug research process.Various chromatograms and mass spectral technology used in conjunction are the main flows of present qualitative and quantitative analysis organic chemistry composition; People such as Wang Guangji adopt rapid screening and the evaluation (publication number: CN 101382525A) of high performance liquid chromatogram-ion trap-flight time tandem mass spectrometer to chemical constitution in the traditional Chinese medicine complex system; For organic principle analysis in the autonomic drug provides a kind of fast and convenient method, but the report of analyzing for the inorganic constituents in the autonomic drug also seldom.
Autonomic drug is because of a great variety and have tangible curative effect and a lower spinoff; Therefore the application at clinicing aspect has time-honored characteristics; Yet the complicated organic and inorganic chemical constitution in the autonomic drug is not illustrated as yet, and this is the main bottleneck in autonomic drug effective substance, quality control and the effect pharmacological research.The development of China's autonomic drug at present still is in period in the ascendant, and therefore, the qualitative and quantitative analysis of chemical constitution seems in the autonomic drug research process and be important.Various chromatograms and mass spectral coupling technique are the main flows of present qualitative and quantitative analysis organic chemistry composition; People such as Wang Guangji adopt rapid screening and the evaluation (publication number: CN 101382525A) in medicine organic principle analysis a kind of fast and convenient method be provided, but for nonmetalloid analysis in medicine inorganic constituents rarely have report of high performance liquid chromatogram-ion trap-flight time tandem mass spectrometer to chemical constitution in the traditional Chinese medicine complex system.
Known matrix solid phase dispersion technology (MSPD) is mainly used in Detecting Pesticide (analytical chemistry, 2005,33 (9): 1318-1320); Do not appearing in the newspapers as yet aspect the ion chromatography mensuration, its cardinal principle is that adsorption stuffing and sample are put into the mortar grinding simultaneously, obtains the potpourri of leather hard; Put then and do or low temperature drying; Refill post, use the eluent solvent pillar, determinand is separated with impurity substances.The matrix solid phase that the patent of Zhao Haixiang etc. relates to sulfa drugs in the animal derived food is disperseed a high-performance liquid chromatogram determination method, and (publication number: CN101241114A), but its use still is traditional matrix solid phase dispersion technology.
Because traditional M SPD technology, because of the bottom quantity of sorbent is few, use solvent when treating that measured ion drip washing is to solvent, the partial impurities ion with organism with the drip washing solvent by wash-out, the chromatography of ions peak-to-peak shape that obtains is disorderly, interference measurement; Be prone to cause the ion chromatographic column system failure simultaneously.These have all limited the widespread use of this method in ion chromatography is measured.
Three, summary of the invention
The purpose of this invention is to provide a kind of matrix solid phase and disperse to extract negative ion and chromatography of ions detection method in the medicine; After deionized water drip washing is used in SPE, leacheate is anion-containing extract with plant drug material and solid extracting agent graphitized carbon and the SPE carbon 18 common mixings that grind.Dilute leacheate to desired concn with deionized water, and extract the membrane filtration that this solution uses 0.22 μ m, gained filtrating is liquid to be analyzed.The ion-chromatographic analyzer test
The present invention includes following steps:
1. contain the extraction of anion liquid in the plant drug material
Use deionized water rinsing again 3～5 times after the plant drug material water cleaned, dry or be no more than dry under 60 ℃ to liquid water content at 3-5%, being crushed to granularity is 0.15～0.25mm, it is subsequent use to put into exsiccator.
After plant drug material 0.05g～0.5g and solid extracting agent graphitized carbon 0.04～0.8g and the carbon 18～3g that takes by weighing above-mentioned granularity grinds mixing 3-6min jointly; Naturally dry to liquid water content at 3-5%; Obtain the potpourri of bulk drug and solid extracting agent; Get 0.4～0.5g potpourri solid-phase extraction column of packing into, insert 0.02～0.03g carbon 18, add 8～9mL deionized water drip washing mixture material by the top of extraction column in the SPE column bottom; In solid-phase extraction column, separate and purification, the leacheate of collecting from the bottom of pillar is anion-containing extract the plant drug material.Dilute extract to desired concn with deionized water, and extract the membrane filtration that this solution of 3mL uses 0.22 μ m, the filtrating of gained is extract to be detected.
The structure of described solid-phase extraction column is as shown in Figure 1, and it comprises column jecket 1, sieve plate 2, the potpourri 3 of solid extracting agent and bulk drug, SPE carbon 18.
2. the determination and analysis inorganic anion component time
(1) ion-chromatographic analyzer test condition
Ion chromatograph separating column 250mm * 4mm, guard column 50mm * 4mm, automatic regeneration rejector electric current 24mA; 30 ℃ of chromatographic column column temperatures, 35 ℃ of temperature control electric conductivity detector pond temperature.
The analytical parameters that sets among the present invention: sample size is 25 μ L (extracts to be detected), and flow velocity is 1.5mL/min, and leacheate is that soda mint and the concentration of concentration 2.8mmol/L is the mixed liquor of the sodium carbonate of 3.5mmol/L.
Get the 1mL extract and under the above-mentioned parameter that sets, carry out the negative ion detection according to the ion chromatography process flow diagram in the accompanying drawing 2.That is: the leacheate in the drip washing bottle 1 is delivered in the sampling valve 3 through pump 2 and is delivered in guard column 4 and the separating column 5 with extract to be analyzed; Negative ion to different separates; Reduce the background conduction through big rejector; Improve sensitivity, and with detection cell 7,8 pairs of negative ion of detecting device detect.
(2) result: the seven kinds of inorganic anion F that survey
-, Cl
-, NO
2 -, Br
-, NO
3 -, PO
4 3-And SO
4 2-In 0.4～12mg/L scope, have good linear relationship, detect and be limited to 1.20～5.00 μ g/L.Its recovery of standard addition is 70%～98%, and precision is 2.09%～5.87%.
The advantage of comparing with known technology
1, anionic separation can be accomplished with purification simultaneously in the autonomic drug extract.Packing layer is improved; (upper strata is the potpourri of bulk drug and solid extracting agent to use double-deck spreading agent; Lower floor is a SPE carbon 18) technology extraction and purification; Promptly on extraction plate, put into a certain amount of adsorbent, purify when having avoided drip washing and not exclusively damage ion chromatographic separation post and interference measurement;
2. the matrix solid phase disperses to extract chromatography of ions detection method accurately comprehensively analysis under the chromatographic condition of the best of 7 kinds of common inorganic anions;
3. this method does not have strict restriction to the kind of autonomic drug.
Four, description of drawings
Fig. 1 is the structural drawing of solid-phase extraction column, and 1 is column jecket among the figure, and 2 is sieve plate, and 3 is the potpourri of solid extracting agent and bulk drug, and 4 is SPE carbon 18.
Fig. 2 is the ion chromatography process flow diagram of inorganic anion, and 1 is leacheate among the figure, and 2 is pump, and 3 is sampling valve, and 4 is guard column, and 5 is separating column, and 6 is rejector, and 7 is detection cell, and 8 is detecting device.
Five, embodiment
Embodiment one:
The extraction of inorganic anion detects in the 1 Herba Hyperici Patuli bulk drug
Use deionized water rinsing again 3 times after Herba Hyperici Patuli bulk drug water cleaned, 60 ℃ dry to liquid water content be 3%, comminutor grind to granularity be 0.15-0.25mm, it is subsequent use to put into exsiccator.
After Herba Hyperici Patuli bulk drug 0.1g and graphitized carbon 0.8g and SPE carbon 18 0.3g that take by weighing above-mentioned granularity grind mixing 3min jointly; Naturally dry to liquid water content be 3%, obtain the potpourri of bulk drug and solid extracting agent, get the 0.5g potpourri solid-phase extraction column of packing into; Its bottom has been inserted carbon 18 0.02g; Top by extraction column adds 8mL deionized water drip washing raw material, collects leacheate from the bottom of extraction column, obtains anion-containing extract.Dilute leacheate to 100mL with deionized water, and extract the membrane filtration that this solution of 3mL uses 0.22 μ m, gained filtrating is extract to be detected.
2, chromatography of ions detects
(1) ion-chromatographic analyzer test condition
With the Dionex ICS1500 of U.S. Dai An company ion chromatograph, Chromeleon6.0 chromatographic work station, IonPac AS14 separating column 250mm * 4mm; IonPac AG14 guard column 50mm * 4mm, ASRS-300 automatic regeneration rejector electric current 24mA, 30 ℃ of chromatographic column column temperatures; 35 ℃ of DS6 temperature control electric conductivity detector detected temperatures; Sample size 25 μ L, flow velocity 1.5mL/min, leacheate are the mixed liquor of 2.8mmol/L soda mint and 3.5mmol/L sodium carbonate.
Get 1mL extract to be analyzed and under the above-mentioned analytical parameters that sets, carry out anion analysis according to the ion chromatography process flow diagram in the accompanying drawing 2.
(2) measure the result: the seven kinds of inorganic anion F that survey
-, Cl
-, NO
2 -, Br
-, NO
3 -, PO
4 3-And SO
4 2-In 0.4～12mg/L scope, have good linear relationship, detect and be limited to 2 μ g/L.Its recovery of standard addition is 80%, and precision is 3%.
Embodiment 2: the extraction of inorganic anion and detection in the purpleback murdannia herb bulk drug
With bulk drug dry to liquid water content be 5%, being crushed to granularity is 0.15-0.25mm, it is subsequent use to put into exsiccator; Take by weighing bulk drug 0.12g and the solid extracting agent graphitized carbon 0.1g and SPE carbon 18 0.7g of above-mentioned granularity; Behind the common grinding mixing 6min, dry naturally, obtain the potpourri of bulk drug and solid extracting agent; Get the 0.4g potpourri solid-phase extraction column (bottom has been inserted 0.03g carbon 18) of packing into; Top by solid-phase extraction column adds 9mL deionized water drip washing raw material, collects leacheate from the bottom of pillar, obtains anion-containing extract; Dilute leacheate to 100m with deionized water, and extract the membrane filtration that this solution of 3mL uses 0.22 μ m, the extract that gained is to be detected.
2, ion chromatography
(1) ion-chromatographic analyzer test condition: identical with example 1.Get the 1mL extract and under the above-mentioned analytical parameters that sets, carry out anion analysis according to the ion chromatography process flow diagram in the accompanying drawing 2.
(2) measure the result: the seven kinds of inorganic anion F that survey
-, Cl
-, NO
2 -, Br
-, NO
3 -, PO
4 3-And SO
4 2-In 0.4～12mg/L scope, have good linear relationship, detect and be limited to 5. μ g/L.Its recovery of standard addition is 91%, and precision is 4.6%.
Claims (3)
1. a matrix solid phase disperses to extract negative ion and chromatography of ions detection method in the medicine, and it is characterized in that: it may further comprise the steps:
1), contains the extraction of anion liquid in the plant drug material
Use deionized water rinsing again 3～5 times after the plant drug material water cleaned, dry or be no more than dry under 60 ℃ to liquid water content at 3-5%, being crushed to granularity is 0.15～0.25mm, it is subsequent use to put into exsiccator; After plant drug material 0.05g～0.5g and solid extracting agent graphitized carbon 0.04～0.8g and the carbon 18～3g that takes by weighing above-mentioned granularity grinds mixing 3-6min jointly; Naturally dry to liquid water content at 3-5%; Obtain the potpourri of plant drug material and solid extracting agent, get 0.4～0.5g potpourri solid-phase extraction column of packing into, insert 0.02～0.03g carbon 18 in the SPE column bottom; Top by extraction column adds 8～9mL deionized water drip washing mixture material; In solid-phase extraction column, separate and purification, the leacheate of collecting from the bottom of pillar is anion-containing extract the plant drug material, dilutes extract to desired concn with deionized water; And extract the membrane filtration that this solution of 3mL uses 0.22 μ m, the filtrating of gained is extract to be detected;
The structure of said solid-phase extraction column comprises column jecket 1, sieve plate 2, the potpourri 3 of solid extracting agent and bulk drug, SPE carbon 18;
2), the determination and analysis inorganic anion component time
(1), ion-chromatographic analyzer test condition
Ion chromatograph separating column 250mm * 4mm, guard column 50mm * 4mm, automatic regeneration rejector electric current 24mA, 30 ℃ of chromatographic column column temperatures, 35 ℃ of temperature control electric conductivity detector pond temperature; Sample size is 25 μ L, and flow velocity is 1.5mL/min, and leacheate is that soda mint and the concentration of concentration 2.8mmol/L is the mixed liquor of the sodium carbonate of 3.5mmol/L;
(2), testing process: the leacheate in the drip washing bottle (1) is delivered in the sampling valve (3) through pump (2) and is delivered in guard column (4) and the separating column (5) with extract to be detected; Negative ion to different separates; Reduce the background conduction through rejector (6); Improve sensitivity, and with detection cell (7), detecting device (8) detects to negative ion.
2. matrix solid phase according to claim 1 disperses to extract negative ion and chromatography of ions detection method in the medicine, and it is characterized in that: said autonomic drug is Herba Hyperici Patuli or purpleback murdannia herb.
3. matrix solid phase according to claim 1 disperses to extract negative ion and chromatography of ions detection method in the medicine, and it is characterized in that: said ion chromatograph is a U.S. Dai An company ion chromatograph.
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Cited By (4)
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| CN106198169A (en) * | 2016-09-21 | 2016-12-07 | 上海市食品药品检验所 | The extraction separation method of the synthetic acidic pigment illegally added in a kind of Chinese crude drug and method for quick |
| CN106918667A (en) * | 2015-12-25 | 2017-07-04 | 北京大学 | The micro- extraction equipment of one kind pressurization and the micro- extracting method of pressurization and its application |
| CN108760916A (en) * | 2018-05-23 | 2018-11-06 | 华南理工大学 | Method that is a kind of while detecting perchlorate and bromate in food |
| CN108828078A (en) * | 2018-03-15 | 2018-11-16 | 云南中烟工业有限责任公司 | The measuring method of inorganic anion in a kind of tobacco gene editor material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106918667A (en) * | 2015-12-25 | 2017-07-04 | 北京大学 | The micro- extraction equipment of one kind pressurization and the micro- extracting method of pressurization and its application |
| CN106918667B (en) * | 2015-12-25 | 2020-08-21 | 北京大学 | Pressurized micro-extraction equipment, pressurized micro-extraction method and application thereof |
| CN106198169A (en) * | 2016-09-21 | 2016-12-07 | 上海市食品药品检验所 | The extraction separation method of the synthetic acidic pigment illegally added in a kind of Chinese crude drug and method for quick |
| CN108828078A (en) * | 2018-03-15 | 2018-11-16 | 云南中烟工业有限责任公司 | The measuring method of inorganic anion in a kind of tobacco gene editor material |
| CN108760916A (en) * | 2018-05-23 | 2018-11-06 | 华南理工大学 | Method that is a kind of while detecting perchlorate and bromate in food |
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Application publication date: 20120718 |