CN106610394A - The preparation of the carbon paste electrode of organic and inorganic biphenyl mesoporous material doping and the Electrochemical Detection for metronidazole - Google Patents
The preparation of the carbon paste electrode of organic and inorganic biphenyl mesoporous material doping and the Electrochemical Detection for metronidazole Download PDFInfo
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- CN106610394A CN106610394A CN201510707244.8A CN201510707244A CN106610394A CN 106610394 A CN106610394 A CN 106610394A CN 201510707244 A CN201510707244 A CN 201510707244A CN 106610394 A CN106610394 A CN 106610394A
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Abstract
The present invention relates to the method that a kind of organic mesoporous material carbon paste electrode of biphenyl detects metronidazole.The 4,4'- bis- of 3.64 mL（Three ethoxy silicon substrates）Biphenyl（BTEBP）, the cetyl trimethylammonium bromide (CTAB) of 3.72 g, the NaOH of 3.88 g and 150 mL deionized waters, 24 hours are stood after ultrasound under the conditions of 100 DEG C, solid is filtered to obtain, hydrochloric acid goes template, be dried to obtain the organic mesoporous material of biphenyl of white（Biphenyl-PMO）.Graphite powder, biphenyl-PMO press 90：10 ground and mixeds are uniform, make the carbon paste electrode of mesoporous material doping.With the carbon paste electrode of biphenyl-PMO modifications as working electrode, platinum electrode be as reference electrode to electrode, Ag/AgCl electrodes, it is established that the differential pulse electrochemical analysis method of metronidazole medicine.When the concentration of metronidazole is 3 × 10-9 Mol/L, pH value of solution can obtain maximum current response on biphenyl modified electrode when being 9.0.The carbon paste electrode of biphenyl-PMO modifications shows wide prospect in terms of the Electrochemical Detection of nitre azole drug, and the fast electrochemical for nitre azole drug detects the method for providing a simplicity.
Description
Technical field
The present invention relates to a kind of electrochemical sensor for determining metronidazole.
Background technology
Metronidazole is a kind of nitroimidazole antibiotics, it is called metronidazole, flagyl, MET, Metronidazole, there is killing action to anaerobe, the metabolin that it is generated when reducing in human body is also acted on anaerobe resistant, suppress the synthesis of the DNA of bacterium, so as to disturb growth, the breeding of bacterium, finally cause bacterial death, anaerobe resistant it is general including：Bacteroides fragilis, fusiform bacilarmature（Because thalli morphology two ends are sharply gained the name in fusiformis）, clostridium tetani, peptococcus, peptostreptococcus, giardia lamblia stiles bacterium.It is initially used to treat trichomoniasis, clinical effectiveness highly significant.Later it has been found that metronidazole can also kill the anaerobic bacteria for causing mouth infection, the specific medicament for anti anaerobic bacteria infection being defined as by the World Health Organization in 1978 is widely used in preventing and treating oral cavity anaerobium infection.It is also frequently used to prevent and treat because of the microbial respiratory tract of anaerobism, alimentary canal, abdominal cavity and pelvic infection, skin soft tissue and bone joint infection in hospital's this product, heart film is scorching, the treatment of septicemia and brain.The level for detecting internal dopamine as can be seen here is of great significance.Electroanalytical Chemistry is widely used in the detection of the Direct Electrochemistry of living matter due to having the advantages that sensitivity is high, the selective good, response time is short, required instrument and equipment is cheap.High sensitivity is developed, the electrochemical sensor for determining metronidazole causes the research interest of people.
Beyond the features such as organic and inorganic mesoporous material has higher specific surface area, big pore volume, regular duct and homogeneous aperture, there is controllability also in terms of the suppleness and parent/hydrophobicity of material, while new activated centre can be derived.Organic and inorganic mesoporous material is located in the skeleton of material due to organic group, and is evenly distributed, therefore will not block duct, and pore volume will not be reduced.There is higher superior function relative to the rear grafting hybrid organic-inorganic mesoporous material that together condensation methods synthesize, this unique characteristic electron will make it be expected to become novel sensor device.
The content of the invention
The present invention is aiming at the problems referred to above and provides a kind of high sensitivity, high selectivity measure of carbon paste electrode of organic and inorganic biphenyl mesoporous material doping for metronidazole.
The preparation of organic and inorganic biphenyl mesoporous material of the present invention：With cationicsurfactants as template, 4,4'- bis-（Three ethoxy silicon substrates）Biphenyl is organic silicon source, in the case of NaOH adjusts pH value, biphenyl-PMO crude products are prepared, then the ethanol solution through filtration, washing and using hydrochloric acid removes template agent removing, the white powder for obtaining is biphenyl-PMO, finally determines the sign spectral line of biphenyl-PMO materials.
The preparation of organic and inorganic biphenyl mesoporous material doping carbon paste electrode of the present invention：Graphite powder, biphenyl-PMO press 90：10 ground and mixeds are uniform, plus 5～6 drop silicone oil further grind, and ground powdered graphite is put in the glass tube of 8cm, insert conductive copper wire.
The method have the characteristics that detecting metronidazole by preparing the carbon paste electrode of organic and inorganic biphenyl mesoporous material doping.On the one hand in order duct can adsorb dopamine to organic and inorganic biphenyl mesoporous material, another aspect organo-functional group can again interact between metronidazole, strengthen electric signal, therefore the carbon paste electrode adulterated with organic and inorganic biphenyl mesoporous material is determined metronidazole and has high sensitivity.
Description of the drawings
Fig. 1 is the sign spectral line of biphenyl-PMO materials；
Fig. 2 is electrochemical response of the metronidazole solution on different modifying electrode（1- blank electrodes, the carbon paste electrode of 2- biphenyl-PMO modifications, the carbon paste electrode of 3-MCM-41 modifications, the carbon paste electrode of 4-Co-SBA-15 modifications）；
Fig. 3 is impact of the metronidazole present to differential pulse, and concentration is 3 × 10-A mol/L（A=4、5、6、7、8、9、10、11、12）.
Specific embodiment
Embodiment 1：The preparation of the organic mesoporous material of biphenyl
With cationicsurfactants as template, BTEBP is organic silicon source, in the case of NaOH adjusts pH value, prepares biphenyl-PMO（Order mesoporous organic material）.Comprise the following steps that：3.72 g CTAB are added in 100 mL round-bottomed flasks, 3.88 g NaOH, add 150 mL deionized waters, 60 DEG C of magnetic agitations 1 hour, after solid is completely dissolved, it is cooled to room temperature, under the conditions of strong agitation, the mL of BTEBP 3.64 are slowly added dropwise, then round-bottomed flask is placed in ultrasonically treated 20 minutes in ultrasonic cleaner, then be stirred at room temperature 24 hours, 24 hours are stood in 100 DEG C of oil baths, obtain white precipitate, the as crude product of biphenyl-PMO, Jing is filtered, washing and template remove biphenyl bridged bond order mesoporous organosilicon material.
Go the operation of template agent removing：Template agent removing is removed in ratio solvent extraction according to 1.00 g crude products, 250 mL absolute ethyl alcohols of correspondence and 9 g hydrochloric acid.Extraction conditions is：Stir 5 hours under 70 DEG C of oil baths, reduce pressure suction filtration, and the biphenyl-PMO of white is obtained after natural drying.
Embodiment 2：The preparation of bare electrode
The 1.0 g graphite powders that weigh with scale are put in agate mortar and are ground, carry out toward the direction as far as possible in process of lapping, 5～6 are added dropwise when seeing that graphite powder is no longer tiny powdery and drip silicone oil, proceed grinding, also to carry out toward the direction as far as possible when regrinding, to avoid graphite powder due to firmly excessive simultaneously, take out of outside mortar.When the graphite powder in finding mortar is presented good sheet, stop grinding, ground powdered graphite is put into into five millimeters of internal diameter, in the glass tube of long 8 cm, it is compacted with thin glass bar, is inserted copper wire, it is using pan paper that the other end polishing of electrode is bright, it is stand-by.
Embodiment 3：The preparation of biphenyl-PMO modified electrodes
Weigh with scale 0.9 g graphite powders, 0.1 g biphenyl-PMO are put in agate mortar and are ground, carry out toward the direction as far as possible in process of lapping, 5～6 are added dropwise when the white powder biphenyl in seeing graphite powder is almost all covered by graphite powder and drip silicone oil, proceed grinding, also to carry out toward the direction as far as possible when regrinding, while to avoid graphite powder due to firmly excessive, take out of outside mortar.When the graphite powder in finding mortar is presented good sheet, stop grinding, ground powdered graphite is put into into five millimeters of internal diameter, in the glass tube of long 8 cm, it is compacted with thin glass bar, is inserted copper wire, it is using pan paper that the other end polishing of electrode is bright, it is stand-by.
Embodiment 4：BR（Britton-Robinson）The preparation of cushioning liquid
The mol/L phosphoric acid of use 0.04 of BR cushioning liquid, boric acid and acetic acid are formulated, and required pH value is adjusted on pH meter with 0.2 mol/L NaOH solutions when using.
The preparation of 0.04 mol/L phosphoric acid, boric acid and acetic acid：1.96 g phosphoric acid, 1.24 g boric acid and 1.20 g acetic acid are weighed respectively, is poured in same 500 mL volumetric flasks after being diluted with secondary water, then be diluted to scale with secondary water, shake up, it is standby.
The preparation of 0.2 mol/L NaOH solutions：2.0 gNaOH solids are weighed, with pouring into after secondary water dissolves in 250 ml volumetric flasks, then scale is diluted to secondary water, shaken up, it is standby.
Nitration mixture is mixed with NaOH solution, is adjusted with pH meter, the BR cushioning liquid that pH value is 3,4,5,6,7,8,9,10 is obtained respectively.
Embodiment 5：The preparation of metronidazole solution
3×10-3Mol/L metronidazole solutions：0.0514 g metronidazoles are weighed with assay balance, with pouring into after secondary water dissolves in 100 mL volumetric flasks, then scale is diluted to secondary water, shaken up, obtain 3 × 10-3The metronidazole solution of mol/L.
3×10-4Mol/L metronidazole solutions：5 mL above-mentioned 3 × 10 are pipetted with pipette-3The metronidazole solution of mol/L, in moving into 50 mL volumetric flasks, with secondary water scale is diluted to, and is shaken up, and obtains 3 × 10-4The metronidazole solution of mol/L.
3×10-5Mol/L metronidazole solutions：The above-mentioned metronidazole solutions of 5 mL are pipetted with pipette, in moving into 50 mL volumetric flasks, with secondary water scale is diluted to, shaken up, obtain 3 × 10-5The metronidazole solution of mol/L.
3×10-6Mol/L metronidazole solutions：The above-mentioned metronidazole solutions of 5 mL are pipetted with pipette, in moving into 50 mL volumetric flasks, with secondary water scale is diluted to, shaken up, obtain 3 × 10-6The metronidazole solution of mol/L.
3×10-7Mol/L metronidazole solutions：The above-mentioned metronidazole solutions of 5 mL are pipetted with pipette, in moving into 50 mL volumetric flasks, with secondary water scale is diluted to, shaken up, obtain 3 × 10-7The metronidazole solution of mol/L.
3×10-8Mol/L metronidazole solutions：The above-mentioned metronidazole solutions of 5 mL are pipetted with pipette, in moving into 50 mL volumetric flasks, with secondary water scale is diluted to, shaken up, obtain 3 × 10-8The metronidazole solution of mol/L.
3×10-9Mol/L metronidazole solutions：The above-mentioned metronidazole solutions of 5 mL are pipetted with pipette, in moving into 50 mL volumetric flasks, with secondary water scale is diluted to, shaken up, obtain 3 × 10-9The metronidazole solution of mol/L.
3×10-10Mol/L metronidazole solutions：The above-mentioned metronidazole solutions of 5 mL are pipetted with pipette, in moving into 50 mL volumetric flasks, with secondary water scale is diluted to, shaken up, obtain 3 × 10-10The metronidazole solution of mol/L.
3×10-11Mol/L metronidazole solutions：The above-mentioned metronidazole solutions of 5 mL are pipetted with pipette, in moving into 50 mL volumetric flasks, with secondary water scale is diluted to, shaken up, obtain 3 × 10-11The metronidazole solution of mol/L.
Metronidazole solution must now match somebody with somebody when using.
Embodiment 6 ：Electrochemical response of the metronidazole on different modifying electrode
Metronidazole solution concentration is with 3 × 10-5 mol/L。
Take BR cushioning liquid（pH=8.0）27 mL, then take 3 × 10-5 The mL of metronidazole solution 3 of mol/L, BR cushioning liquid（V）：Metronidazole solution（V）= 9:1, by mixed solution as small beaker in, the oxygen in leading to the min of nitrogen 10 to remove solution determines electrochemical response of the metronidazole solution on different modifying electrode, record data with differential pulse method.
Parameter setting：The V of initial point position -0.7, terminates the V of current potential 0.0, the V of current potential increment 0.004, the V of impulse amplitude 0.08, the s of pulse width 0.03, the s of pulse spacing 0.1, the s of stand-by period 2.
Embodiment 7 ：Determine the electrochemical response of variable concentrations metronidazole
Take BR cushioning liquid（pH=8.0）27 mL, take the mL of metronidazole solution 3 of 3 × 10-3 mol/L again, by mixed solution as small beaker in, lead to the min of nitrogen 10 to remove solution in oxygen, electrochemical response of the metronidazole solution on biphenyl modified electrode, record data are determined with differential pulse method.
3×10-4 mol/L、3×10-5 mol/L、3×10-6 mol/L、3×10-7 mol/L、3×10-8 mol/L、3×10-9 mol/L、3×10-10 mol/L、3×10-11
The metronidazole solution repeat the above steps of mol/L.
Metronidazole present is as shown in Figure 3 with the linear relationship of peak current.As seen from the figure, metronidazole solution is from 3 × 10-5Mol/L to 3 × 10-9Mol/L concentration ranges, peak current gradually increases, when concentration is from 3 × 10-9Mol/L is reduced to 3 × 10-12During mol/L, peak current is gradually reduced again.3 × 10-9During mol/L, peak current reaches maximum.So it is 3 × 10 that experimentation selects the concentration of metronidazole-9mol/L.Even if the concentration of metronidazole reaches 10-12During mol/L, remain to detect stronger electrochemical signals, it is seen that the carbon paste electrode of biphenyl-PMO modifications can be very good to detect metronidazole for working electrode.
Claims (6)
1. the method for the carbon paste electrode Electrochemical Detection metronidazole of a kind of biphenyl organic mesoporous material doping, it is characterised in that:3.64mL 4,4'- bis- (three ethoxy silicon substrates) biphenyl (BTEBP), the cetyl trimethylammonium bromide (CTAB) of 3.72g, the NaOH of 3.88g and 150mL deionized waters, 24 hours are stood after ultrasound under the conditions of 100 DEG C, filter to obtain solid, hydrochloric acid goes template, is dried to obtain biphenyl-PMO.Graphite powder, biphenyl-PMO press 90：10 ground and mixeds are uniform, make the carbon paste electrode of organic mesoporous material doping.Then the measure of metronidazole is carried out in current potential -0.491V, 0.lmol/L phosphate buffer solutions with electrochemical workstation three-electrode system.
2. the method for the carbon paste electrode Electrochemical Detection metronidazole of the organic mesoporous material doping of a kind of biphenyl as claimed in claim 1, it is characterised in that organic mesoporous material is biphenyl-PMO.
3. the method for the carbon paste electrode Electrochemical Detection metronidazole of the organic mesoporous material doping of a kind of biphenyl as claimed in claim 1, it is characterised in that the hydrophobic organic solvent is silicone oil.
4. the method for the carbon paste electrode Electrochemical Detection metronidazole of the organic mesoporous material doping of a kind of biphenyl as claimed in claim 1, it is characterized in that the NaOH of CTAB, 3.88g of BTEBP, 3.72g of 3.64mL and 150mL deionized waters, 24 hours are stood after ultrasound under the conditions of 100 DEG C, filter to obtain solid, hydrochloric acid goes template, is dried to obtain biphenyl-PMO.
5. the method for the carbon paste electrode Electrochemical Detection metronidazole of the organic mesoporous material doping of a kind of biphenyl as claimed in claim 1, it is characterised in that graphite powder, biphenyl-PMO press 90：10 ground and mixeds are uniform, make the carbon paste electrode of organic mesoporous material doping.
6. a kind of method of the carbon paste electrode Electrochemical Detection dopamine of the organic mesoporous material doping of biphenyl as claimed in claim 1, it is characterised in that test potential -0.491V.
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2015
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| CN102043006A (en) * | 2010-10-29 | 2011-05-04 | 济南大学 | Method for preparing water-soluble quantum dot carbon paste electrode for detecting trace amino acid in food |
| CN102701333A (en) * | 2012-05-31 | 2012-10-03 | 华南师范大学 | Preparation method of Ce (cerium) doped titanium base SnO2 (stannic oxide) electrodes and metronidazole wastewater treatment method |
| CN104897753A (en) * | 2015-02-05 | 2015-09-09 | 石河子大学 | Molecularly-imprinted polymer modified nanometer porous gold-silver alloy wire electrode and application thereof |
| CN104833717A (en) * | 2015-05-07 | 2015-08-12 | 湖北民族学院 | Method of using mesoporous SiO2 to modify carbon paste electrode and measuring magnolol and honokiol at the same time |
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Application publication date: 20170503 |