CN108717002A - A kind of method of galanthamine in detection Lycoris aurea - Google Patents
A kind of method of galanthamine in detection Lycoris aurea Download PDFInfo
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- CN108717002A CN108717002A CN201810541070.6A CN201810541070A CN108717002A CN 108717002 A CN108717002 A CN 108717002A CN 201810541070 A CN201810541070 A CN 201810541070A CN 108717002 A CN108717002 A CN 108717002A
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Abstract
The present invention discloses a kind of method detecting galanthamine in Lycoris aurea.This method be related to plant sample processing, nanogold print electrode sensor preparation and Electrochemical Detection.The decorated by nano-gold sensor that prints electrode fully is adsorbed in sample extraction liquid, the nanogold sensor that prints electrode then is done into differential pulse voltammetry scanning, measures oxidation peak current value.In detectable range, galanthamine content and oxidation peak current intensity are in a linear relationship in the Lycoris aurea of sensor absorption, according to working curve, can calculate the content of galanthamine in sample to be tested.Decorated by nano-gold prepared by the present invention prints electrode sensor by nanotechnology and screen printing technique combination, is remarkably improved sensor and can reach 0.013 μM to the sensitivity of galanthamine Concentration Testing and minimum detection limit in Lycoris aurea.
Description
Technical field
The present invention relates to the methods of galanthamine in detection Lycoris herbage flower Lycoris aurea, and in particular to arrives a kind of nanometer
The method that gold modifies the detection galanthamine that prints electrode.
Background technology
Lycoris aurea is the perennial herbage flower of Lycoris, be grown on more it is shady and cool be protected from light place, it is warm-natured, taste put down it is sweet, have detumescence,
Medicinal powder for relieving pain poison, emetic and other effects.Galanthamine is a kind of Lycoris aurea secondary metabolite alkaloid, is distributed mainly on its bulb
In,《Chinese Pharmacopoeia》The middle injection for having recorded galanthamine hydrobromide and tablet can be used for treating caused by nervous system disease
Feel or dyskinesia, including sequelae of infantile paralysis, myasthenia gravis, the treatment of enteroparalysis and as anti-curare class drug and
Analeptic etc. after surgery anesthesia.In recent years, galanthamine hydrobromide has been used as acetylcholinesterase inhibitor, by domestic external application
In the treatment of mild to moderate Alzheimer syndrome.
It is the instrumental methods such as chromatography, mass spectrum that substance, which detects most widely used method, in plant at present, which can
Test substance is fast and accurately quantitatively detected under conditions of using a small amount of sample, but this kind of detection means needs complexity
Pretreatment process, expensive special instrument and skilled operator, it is difficult to meet real-time, online detection requirements.Electrification
It is a kind of simple, quick, high sensitivity detection method, Iranian scholar (Journal of to learn detection technique
Electroanalytical Chemistry 785(2017):220-228.) succeeded realizes Garland on glass-carbon electrode
His quick detection, detection is limited to 0.18 μM, but glass-carbon electrode needs polishing in advance, and electrolytic cell is needed to be detected operation, limit
It makes it and is only applicable to test in laboratory.Based on the electrochemical assay to print electrode as a kind of novel Fast Detection Technique, energy
It is enough that the plant sample after simple pre-treatment is detected, with fast and convenient, portable, easy micromation etc. is excellent at a low price
Point.However since the self performance that prints electrode is limited, this method haves the shortcomings that sensitivity is not high, so that it cannot be used for Garland
His quick direct detection.
Nanogold is a kind of small gold particle of diameter in 1-100nm, has that preparation method is simple, adsorption ability is excellent
It is different, electric conductivity is strong, chemical state stablize the features such as, can improve electronics transfer to printing electrode to modify using nanogold
Rate and electrode response speed.
Invention content
The purpose of the present invention is in view of the deficiencies of the prior art, it is proposed that one kind is simple in structure, easy to use, price is low
The rapid decorated by nano-gold of honest and clean, high sensitivity, detection process prints electrode sensor for detecting Lycoris herbaceous plant suddenly
Laugh at the method for middle galanthamine content.
The present invention relates to plant sample processing, nanogold print electrode sensor preparation and Electrochemical Detection, specifically
It is：
The processing of step (1) plant samples：After Lycoris aurea bulb is shredded, blended to slurry using clean food blending machine
Paste weighs in sample to centrifuge tube, while a certain amount of methanol is added, and is positioned over after lid upper tube cap in ultrasonic machine and carries out ultrasonic extraction
It takes；Gained dispersion liquid obtains plant sample extracting solution after filtering.
Step (2) decorated by nano-gold prints electrode the preparation of sensor：It will print electrode and carry out surface clean.It will cleaning
Printing electrode afterwards is placed in the obtained decorated by nano-gold printing of progress constant potential electro-deposition in the mixed solution of dilute hydrochloric acid and gold chloride
Electrode sensor.
The drafting of step (3) standard curves：Mother liquor made of galanthamine solid is weighed, phosphoric acid is added by gradient capacity
The standard solution to be measured of gradient concentration is obtained in buffer solution, after constant volume.The decorated by nano-gold sensor that prints electrode is sequentially inserted into
Various concentration galanthamine standard mother liquor fully carries out scan round, using being surveyed after absorption in 0.5-1.5V current ranges
Oxidation peak current value draws standard working curve, and calculates linear equation.
The detection of galanthamine in step (4) Lycoris aurea：The above decorated by nano-gold sensor that prints electrode is carried in sample
It takes in liquid and fully adsorbs, the nanogold sensor that prints electrode then is done into differential pulse voltammetry scanning, measures oxidation peak current
Value.In detectable range, galanthamine content and oxidation peak current intensity are in a linear relationship in the Lycoris aurea of sensor absorption,
According to working curve, the content of galanthamine in sample to be tested can be calculated.
Preferably, the plant sample amount in step (1) is 1-10g, methanol 5-20mL.
Preferably, ultrasonic power is 200-500W, supersonic frequency 20kHz in step (1).
Preferably, the material of filter paper is polyether sulfone in step (1), and aperture is 200nm-2 μm.
Preferably, print electrode as screen printing electrode, it is described print electrode in be integrated with working electrode, reference electrode and
Auxiliary electrode.Described print electrode is a kind of low-cost disposable electrode, is very suitable for quickly detecting.
Preferably, described to print electrode through NDK Noguchis bus, hole hole plate and Du Pont's line and transmission connection of printing electrode.
Preferably, in step (2) electrolyte dilute sulfuric acid a concentration of 0.1M-0.5M.
Preferably, in step (2) gold chloride a concentration of 0.1wt%-0.5wt%.
Preferably, electro-deposition current potential is+0.4-0.5V in step (2).
Preferably, electrodeposition time is 1-5min in step (2).
The invention has the advantages that：
1. the present invention, without being purified and being concentrated, substantially reduces sample in Lycoris aurea specimen sample pretreatment process
The time required to processing.
2. decorated by nano-gold prepared by the present invention prints electrode, sensor combines nanotechnology and screen printing technique, can
It significantly improves sensor and 0.013 μM can reach to the sensitivity of galanthamine Concentration Testing and minimum detection limit in Lycoris aurea.
Specific implementation mode
With reference to specific embodiment, the present invention is further analyzed.
Embodiment 1.
The detection method of galanthamine, operating procedure are as follows in a kind of Lycoris aurea：
(1) sample process：After Lycoris aurea bulb is shredded, blended to starchiness using clean food blending machine, by sample
Product weigh in 10g to 50mL centrifuge tubes, addition 20mL methanol, are positioned in ultrasonic machine after upper tube cap after lid upper tube cap and carry out ultrasound
Extract 10min, ultrasonic power 200W, supersonic frequency 20kHz.Gained dispersion liquid passes through the apertures 200nm polyether sulfone filter paper mistake
Lycoris aurea extracting solution is obtained after filter.
(2) decorated by nano-gold prints electrode the preparation of sensor：It is respectively washed surface of printing electrode with distilled water and ethyl alcohol,
By printing electrode as in the mixed solution of 20mL dilute hydrochloric acid (0.1M) and gold chloride (0.1wt%) after cleaning, in+0.4V electricity
Pressure carries out constant potential electro-deposition 1min decorated by nano-gold is made printing electrode sensor.
(3) drafting of standard curve：Mother liquor made of galanthamine solid is weighed, is configured to methanol dilution, constant volume dense
Degree is the mother liquor of 0.1mM, takes a certain amount of mother liquor that the phosphate buffer of 0.1mM pH=7.0 is added respectively, is added after constant volume
Lan Tamin gradient concentrations are followed successively by 0.1 μM, 0.2 μM, 0.4 μM, 0.8 μM and 1.0 μM of standard solution to be measured.
(4) in Lycoris aurea galanthamine detection：By the above decorated by nano-gold print electrode sensor immerse sample extraction
It is fully adsorbed in liquid, differential pulse voltammetry scanning, detection oxidation is carried out in 0.5-1.5V using CH1760b electrochemical workstations
Peak current intensity.Differential pulse voltammetry scanning gained oxidation peak to peak current is with galanthamine concentration within the scope of 0.1-1.0 μM
Detection in a linear relationship is limited to 0.05 μM.
Embodiment 2.
The detection method of galanthamine, operating procedure are as follows in a kind of Lycoris aurea：
(1) sample process：After Lycoris aurea bulb is shredded, blended to starchiness using clean food blending machine, by sample
Product weigh in 5g to 50mL centrifuge tubes, addition 10mL methanol, are positioned in ultrasonic machine after upper tube cap after lid upper tube cap and carry out ultrasound
10min is extracted, gained dispersion liquid obtains Lycoris aurea extracting solution after 2 μm of aperture polyether sulfone filter paper filterings.
(2) decorated by nano-gold prints electrode the preparation of sensor：It is respectively washed surface of printing electrode with distilled water and ethyl alcohol,
By printing electrode as in the mixed solution of 20mL dilute hydrochloric acid (0.2M) and gold chloride (0.5wt%) after cleaning, in+0.5V electricity
Pressure carries out constant potential electro-deposition 5min decorated by nano-gold is made printing electrode sensor.
(3) drafting of standard curve：Mother liquor made of galanthamine solid is weighed, is configured to methanol dilution, constant volume dense
Degree is the mother liquor of 0.1mM, takes a certain amount of mother liquor that the phosphate buffer of 0.1mM pH=7.0 is added respectively, is added after constant volume
Lan Tamin gradient concentrations are followed successively by 0.05 μM, 0.1 μM, 0.5 μM, 1.0 μM and 2.0 μM of standard solution to be measured.
(4) in Lycoris aurea galanthamine detection：By the above decorated by nano-gold print electrode sensor immerse sample extraction
It is fully adsorbed in liquid, carrying out differential pulse voltammetry in 0.5-1.5V current ranges using CH1760b electrochemical workstations sweeps
It retouches, detects oxidation peak current intensity.Differential pulse voltammetry scanning gained oxidation peak to peak current is with galanthamine concentration in 0.05-
In a linear relationship within the scope of 2.0 μM, detection is limited to 0.013 μM.
The description of above-described embodiment is in order to illustrate and illustration purpose, and is to explain the principle of the present invention and practical application,
It is not the limitation for the present invention, the present invention is not limited only to above-described embodiment, as long as meeting, the present invention claims belong to this
The protection domain of invention.
Claims (9)
1. a kind of method of galanthamine in detection Lycoris aurea, it is characterised in that this approach includes the following steps：
The processing of step (1) plant samples：
After Lycoris aurea bulb is shredded, is blended to starchiness, weighed in sample to centrifuge tube, together using clean food blending machine
When a certain amount of methanol is added, be positioned over after lid upper tube cap in ultrasonic machine and carry out ultrasonic extraction；Gained dispersion liquid obtains after filtering
To plant sample extracting solution；
Step (2) decorated by nano-gold prints electrode the preparation of sensor：
It will print electrode and carry out surface clean；By printing electrode after cleaning be placed in the mixed solution of dilute hydrochloric acid and gold chloride into
Row constant potential electro-deposition is made decorated by nano-gold and prints electrode sensor；
The drafting of step (3) standard curves：
Mother liquor made of galanthamine solid is weighed, is added in phosphate buffer by gradient capacity, gradient concentration is obtained after constant volume
Standard solution to be measured；The decorated by nano-gold sensor that prints electrode is sequentially inserted into various concentration galanthamine standard mother liquor, is filled
Scan round is carried out in 0.5-1.5V current ranges after dividing absorption, it is bent to draw standard work using institute's oxygen determination peak point current
Line, and calculate linear equation；
The detection of galanthamine in step (4) Lycoris aurea：
The above decorated by nano-gold sensor that prints electrode fully is adsorbed in sample extraction liquid, then nanogold prints electrode
Sensor does differential pulse voltammetry scanning, measures oxidation peak current value；In detectable range, the Lycoris aurea of sensor absorption
Middle galanthamine content and oxidation peak current intensity are in a linear relationship, according to working curve, can calculate in sample to be tested Garland he
Quick content.
2. the method for galanthamine in a kind of detection Lycoris aurea as described in claim 1, it is characterised in that the plant in step (1)
Object sample size is 1-10g, methanol 5-20mL.
3. the method for galanthamine in a kind of detection Lycoris aurea as described in claim 1, it is characterised in that ultrasonic in step (1)
Power is 200-500W, supersonic frequency 20kHz.
4. the method for galanthamine in a kind of detection Lycoris aurea as described in claim 1, it is characterised in that filter paper in step (1)
Material be polyether sulfone, aperture be 200nm-2 μm.
5. the method for galanthamine in a kind of detection Lycoris aurea as described in claim 1, it is characterised in that described to print electrode
Pass through NDK Noguchis bus, hole hole plate and Du Pont's line and transmission connection of printing electrode.
6. the method for galanthamine in a kind of detection Lycoris aurea as described in claim 1, it is characterised in that electrolysis in step (2)
A concentration of 0.1M-0.5M of liquid dilute sulfuric acid.
7. the method for galanthamine in a kind of detection Lycoris aurea as described in claim 1, it is characterised in that chlorine gold in step (2)
A concentration of 0.1wt%-0.5wt% of acid.
8. the method for galanthamine in a kind of detection Lycoris aurea as described in claim 1, it is characterised in that electricity is heavy in step (2)
Product current potential is+0.4-0.5V.
9. the method for galanthamine in a kind of detection Lycoris aurea as described in claim 1, it is characterised in that electricity is heavy in step (2)
The product time is 1-5min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111413392A (en) * | 2020-03-25 | 2020-07-14 | 杭州电子科技大学 | Method for collecting electrochemical spectrum of lycoris seeds |
Citations (3)
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|---|---|---|---|---|
| CN102335297A (en) * | 2010-07-23 | 2012-02-01 | 长春工程学院 | Capillary tube electrophoresis electrochemiluminescence detecting method for galantamine hydrobromide in traditional Chinese medicinal short-tube lycoris extract |
| CN105445356A (en) * | 2015-12-16 | 2016-03-30 | 江南大学 | Portable ractopamine molecular imprinted silk-screen printed electrochemical sensor |
| CN107462656A (en) * | 2017-07-04 | 2017-12-12 | 上海市农业科学院 | A kind of method of galanthamine content in quick detection amrallid |
-
2018
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102335297A (en) * | 2010-07-23 | 2012-02-01 | 长春工程学院 | Capillary tube electrophoresis electrochemiluminescence detecting method for galantamine hydrobromide in traditional Chinese medicinal short-tube lycoris extract |
| CN105445356A (en) * | 2015-12-16 | 2016-03-30 | 江南大学 | Portable ractopamine molecular imprinted silk-screen printed electrochemical sensor |
| CN107462656A (en) * | 2017-07-04 | 2017-12-12 | 上海市农业科学院 | A kind of method of galanthamine content in quick detection amrallid |
Non-Patent Citations (3)
| Title |
|---|
| BIYANG DENG ET AL.: "Determination of galanthamine in Bulbus Lycoridis Radiatae by coupling capillary electrophoresis with end-column electrochemiluminescence detection", 《J. SEP. SCI.》 * |
| MAJID ARVAND ET AL.: "A novel one-step electrochemical preparation of silver nanoparticles/poly(3-methylthiophene) nanocomposite for detection of galantamine in human cerebrospinal fluid and narcissus", 《JOURNAL OF ELECTROANALYTICAL CHEMISTRY》 * |
| 宋伟 等: "纳米金修饰丝网印刷电极检测水中对苯二酚的研究", 《第五届全国环境化学大会会议论文集》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111413392A (en) * | 2020-03-25 | 2020-07-14 | 杭州电子科技大学 | Method for collecting electrochemical spectrum of lycoris seeds |
| CN111413392B (en) * | 2020-03-25 | 2022-05-13 | 杭州电子科技大学 | Method for collecting electrochemical spectrum of lycoris seeds |
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