CN103439395A - Method for fast detecting acetaminophen contained in blood at high sensitivity by utilizing Fe3O4 magnetic nanoparticles - Google Patents
Method for fast detecting acetaminophen contained in blood at high sensitivity by utilizing Fe3O4 magnetic nanoparticles Download PDFInfo
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- CN103439395A CN103439395A CN2013104250622A CN201310425062A CN103439395A CN 103439395 A CN103439395 A CN 103439395A CN 2013104250622 A CN2013104250622 A CN 2013104250622A CN 201310425062 A CN201310425062 A CN 201310425062A CN 103439395 A CN103439395 A CN 103439395A
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Abstract
The invention discloses a method for fast detecting acetaminophen contained in blood at high sensitivity by utilizing Fe3O4 magnetic nanoparticles. An electrode modified by the Fe3O4 magnetic nanoparticles is a working electrode, and the method for detecting the acetaminophen contained in the blood is established by utilizing different current catalysis strength generated by the working electrode on the acetaminophen with the concentration of 0,4, 0.6, 0.8, 1, 4, 8, 20, 40 and 60mu micromoles/L; the scanning potential is 0.3-0.7 V, the scanning speed is 100 mV/s; in an acetic acid-sodium acetate (HAc-NaAc) buffer solution with pH=5.2 and the concentration of 0.03 mol/L, the concentration of the acetaminophen ranges from 4*(10<-7>) mol/L to 6*(10<-5>) mol/L, the concentration and the catalytic current strength of the surface of the electrode are in good linear relationship, and the detection limit is 8.13*(10<-8>) mol/L. The method disclosed by the invention has the advantages of sensitivity, good selectivity and more convenience and easiness for detection on low-concentration acetaminophen.
Description
Technical field
The present invention relates to a kind of Fe of utilization
3o
4the method of the paracetamol in the highly sensitive fast detecting blood of magnetic nano-particle.
Background technology
Paracetamol is used for cat fever, arthralgia, neuralgia, antimigraine, pain caused by cancer and the rear pain relieving of operation etc. as a kind of common medicine.Drink for a long time or while applying other Liver enzyme inducers, especially the patient of barbiturates or other antispasmodics, the danger of hepatotoxicity reaction can occur after using continuously.Therefore being necessary to improve sensitivity on existing basis studies and a kind of paracetamol is had to highly sensitive detection method.Magnetic Fe
3o
4the magnetic particle compound substance has the characteristics such as grain diameter is little, specific surface area large, magnetosensitive, is widely used in the fields such as magnetic memory material, senser element, high density magnetic storage medium, medicine control release.
Summary of the invention
The purpose of this invention is to provide a kind of high sensitivity, high selectivity, the range of linearity is wide, instrument is simple, favorable reproducibility, appearance is manageable that paracetamol in blood is carried out to method for measuring.
Conceive as follows: because the particle diameter of nano particle is very small, just there is small size effectiveness, quantum size effectiveness, surface effect, macro quanta tunnel effect.In nano material, Fe
3o
4the character that magnetic nano-particle is good with it, obtained paying close attention to widely.Fe
3o
4magnetic nano-particle has the characteristics such as grain diameter is little, specific surface area large, magnetosensitive, is widely used in biomedical the detection and catalyst support.Be applied in electrochemical sensor, make specific surface area larger, be more suitable for supported ionic.And utilize Fe
3o
4magnetic nano-particle, make the current-responsive intensity of paracetamol in end liquid increase; Amount by paracetamol in liquid at the bottom of continuous change obtains different current-responsive loudness, and then the content of direct-detection paracetamol.
The present invention utilizes electrochemical process, Fe
3o
4magnetic nano-particle strengthens the strength of current of paracetamol in end liquid, and Determination of Acetaminophen is 4 * 10
-7~ 6 * 10
-5become good linear relationship in the mol/L scope with electrode surface strength of current.
Concrete steps are as follows:
1, the making of glass-carbon electrode:
At long 2 ~ 5 cm, in the glass tube of internal diameter 2 ~ 5 mm, carbon plate is fully contacted with iron core, 1 ~ 3 mm of this iron core diameter, long 3 ~ 7 cm; The glass tube hollow parts fills up with paraffin, plays effect fixing, insulation, by the polishing of electrode carbon plate end surfaces.
2, Fe
3o
4synthesizing of magnetic nano-particle:
Pass into nitrogen 2 ~ 7 minutes with deaeration in 250 mL reaction bulbs, take FeCl
36H
2o and FeSO
47H
2o also makes molysite in molar ratio for n (Fe
3+): n (Fe
2+)=2:1.2 mixes, add water to be dissolved after, it is drained in the reaction bulb that is full of nitrogen; In 50 ℃ of calibration cells, add the NaOH that concentration is 2 mol/L under non-magnetic agitation state, regulator solution pH is 8 ~ 13, then is warming up to 80 ℃ of slakings 0.5 ~ 2 hour, whole reaction is carried out under nitrogen protection; Precipitation is separated through externally-applied magnetic field, and redistilled water cleans 2 ~ 3 times to neutral, is settled to 100 mL volumetric flasks, is kept in 4 ℃ of refrigerators standby.
3, magnetic Fe SO
4the preparation of modified electrode:
Get the Fe that 5 ~ 15 μ L steps (2) make
3o
4magnetic nano-particle, under externally-applied magnetic field, after dropping to the glass-carbon electrode that step (1) handles well, dry rear stand-by.
4, detection method:
The Fe that step (3) is handled well
3o
4the magnetic nano-particle modified electrode is placed in respectively the detection system of the paracetamol that contains 0.4,0.6,0.8,1,4,8,20,40 and 60 μ mol/L, directly measures strength of current; Detection system is: acetic acid-sodium acetate (HAc-NaAc) buffer solution of 0.03 mol/L of 2 ~ 10 mLpH=5.2; Adopt differential pulse voltammetry to be detected it, scanning current potential 0.3 V ~ 0.7 V, sweeping speed is 100 mV/s.
5, the drafting of standard working curve:
0.03 mol/L HAc-NaAc buffer solution (pH=5.2) of the paracetamol that adds respectively 5 mL to contain 0.4,0.6,0.8,1,4,8,20,40 and 60 μ mol/L in 9 beakers, carry out the electrochemical source of current detection; The concentration of paracetamol is 4 * 10
-7~ 6 * 10
-5in the mol/L scope, concentration and strength of current are good linear relationship, and its equation of linear regression is: I=0.212C+9.545, linearly dependent coefficient r=0.999.
The present invention has overcome that prior art exists when detecting that sensitivity is low, sample preparation is complicated, instrument is expensive or the shortcoming such as practical ranges is narrow, has improved better sensitivity and selectivity, simpler for the detection of the paracetamol of low concentration.
The accompanying drawing explanation
Fig. 1 is electrode that the embodiment of the present invention the is different HAc-NaAc buffer solution at 0.03 mol/L of pH=5.2, the differential pulse voltammetry figure that Determination of Acetaminophen is 8 μ mol/L, the wherein naked glass-carbon electrode of a; B is for having modified Fe
3o
4the glass-carbon electrode of magnetic nano-particle.
The graph of a relation of the strength of current that Fig. 2 is embodiment of the present invention Determination of Acetaminophen and electrode surface.
Embodiment
Embodiment:
1, the preparation of glass-carbon electrode:
At long 3 cm, in the glass tube of internal diameter 3 mm, carbon plate is fully contacted with iron core, 1.5 mm of this iron core diameter, long 5 cm; The glass tube hollow parts fills up with paraffin, plays effect fixing, insulation, by the polishing of electrode carbon plate end surfaces.
2, Fe
3o
4synthesizing of magnetic nano-particle:
Pass into nitrogen 5 minutes with deaeration in 250 mL reaction bulbs, taking is n (Fe in molar ratio
3+): n (Fe
2+the FeCl of)=2: 1.2
36H
2o and FeSO
47H
2o also mixes it, add water to be dissolved after, it is drained in the reaction bulb that is full of nitrogen; In 50 ℃ of calibration cells, add 2 mol/L NaOH under non-magnetic agitation state, regulator solution pH is after 10, pH remains unchanged, then is warming up to 80 ℃ of slakings 1 hour, whole reaction is carried out under nitrogen protection; Precipitation is separated through externally-applied magnetic field, and redistilled water cleans 2 times to neutral, is settled to 100 mL volumetric flasks, is kept in 4 ℃ of refrigerators standby.
3, magnetic Fe
3o
4the preparation of modified electrode:
Get the Fe that 10 μ L steps (2) make
3o
4magnetic nano-particle, under externally-applied magnetic field, after dropping to the glass-carbon electrode that step (1) handles well, dry rear stand-by.
4, detection method:
The Fe that step (3) is handled well
3o
4the magnetic nano-particle modified electrode is placed in respectively the detection system of the paracetamol that contains 0.4,0.6,0.8,1,4,8,20,40 and 60 μ mol/L, directly measures the intensity of electric current; Detection system is: acetic acid-sodium acetate (HAc-NaAc) buffer solution of 0.03 mol/L of 2 ~ 10 mL pH=5.2; Adopt differential pulse voltammetry to be detected it, scanning current potential 0.3 V ~ 0.7 V, sweeping speed is 100 mV/s.
5, the drafting of standard working curve:
0.03 mol/L HAc-NaAc buffer solution (pH=5.2) of the paracetamol that adds respectively 5 mL to contain 0.4,0.6,0.8,1,4,8,20,40 and 60 μ mol/L in 9 beakers, carry out the electrochemical source of current detection; The concentration of paracetamol is 4 * 10
-7~ 6 * 10
-5in the mol/L scope, concentration and strength of current are good linear relationship, and its equation of linear regression is: I=0.212C+9.545, linearly dependent coefficient r=0.999.
6, the mensuration of Determination Paracetamol in Paracetamol in blood sample:
Because providing in blood serum sample, Hospital of Guilin University of Technology do not detect paracetamol, therefore adopt recovery testu; Get 5 mL blood serum samples, add the saturated (NH of 5 mL
4)
2sO
4solution is in centrifuge tube, and sample, after 8000 rpm centrifugal 20 minutes, is got supernatant and is placed on (pH=7.4) dialysed overnight in phosphate buffered solution; After adding the paracetamol of variable concentrations in serum sample after processing, utilize three-electrode system to be detected liquid to be measured.It is 0.3 V ~ 0.7 V that voltage is set, and sweeping speed is 100 mV/s.Calculate the concentration C of paracetamol according to calibration curve.Calculate recovery rate, result is as shown in table 1.
Table 1: mark-on recovery test data
Claims (1)
1. one kind is utilized Fe
3o
4magnetic nano-particle detects the method for the paracetamol in blood, it is characterized in that concrete steps are:
(1) making of glass-carbon electrode:
At long 2 ~ 5 cm, in the glass tube of internal diameter 2 ~ 5 mm, carbon plate is fully contacted with iron core, 1 ~ 3 mm of this iron core diameter, long 3 ~ 7 cm; The glass tube hollow parts fills up with paraffin, plays effect fixing, insulation, by the polishing of electrode carbon plate end surfaces;
(2) Fe
3o
4synthesizing of magnetic nano-particle:
Pass into nitrogen 2 ~ 7 minutes with deaeration in 250 mL reaction bulbs, take FeCl
36H
2o and FeSO
47H
2o also makes molysite in molar ratio for n (Fe
3+): n (Fe
2+)=2: 1.2 mix, add water to be dissolved after, it is drained in the reaction bulb that is full of nitrogen; In 50 ℃ of calibration cells, add the NaOH that concentration is 2 mol/L under non-magnetic agitation state, regulator solution pH is 8 ~ 13, then is warming up to 80 ℃ of slakings 0.5 ~ 2 hour, whole reaction is carried out under nitrogen protection; Precipitation is separated through externally-applied magnetic field, and redistilled water cleans 2 ~ 3 times to neutral, is settled to 100 mL volumetric flasks, is kept in 4 ℃ of refrigerators standby;
(3) magnetic Fe
3o
4the preparation of modified electrode:
Get the Fe that 5 ~ 15 μ L steps (2) make
3o
4magnetic nano-particle, under externally-applied magnetic field, after dropping to the glass-carbon electrode that step (1) handles well, dry rear stand-by;
(4) detection method:
The Fe that step (3) is handled well
3o
4the magnetic nano-particle modified electrode is placed in respectively the detection system of the paracetamol that contains 0.4,0.6,0.8,1,4,8,20,40 and 60 μ mol/L, directly measures strength of current; Detection system is: acetic acid-sodium acetate of 0.03 mol/L of 2 ~ 10 mL pH=5.2 is HAc-NaAc buffer solution; Adopt differential pulse voltammetry to be detected it, scanning current potential 0.3 V ~ 0.7 V, sweeping speed is 100 mV/s;
(5) drafting of standard working curve:
0.03 mol/L HAc-NaAc buffer solution of the paracetamol that adds respectively 5 mL to contain 0.4,0.6,0.8,1,4,8,20,40 and 60 μ mol/L in 9 beakers, HAc-NaAc buffer solution pH=5.2, carry out the electrochemical source of current detection; The concentration of paracetamol is 4 * 10
-7~ 6 * 10
-5in the mol/L scope, concentration and strength of current are good linear relationship, and its equation of linear regression is: I=0.212C+9.545, linearly dependent coefficient r=0.999.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111458390A (en) * | 2020-04-11 | 2020-07-28 | 石河子大学 | Fe3O4Preparation method and application of modified electrode material |
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|---|---|---|---|---|
| CN101329296A (en) * | 2007-12-20 | 2008-12-24 | 复旦大学 | Glucolase electrode based on magnetic carbon nano-tube and preparation method thereof |
| CN101629931A (en) * | 2009-07-31 | 2010-01-20 | 江苏科技大学 | Anti-ascorbate sensor electrode and preparation method thereof |
| CN101986148A (en) * | 2010-10-18 | 2011-03-16 | 上海市七宝中学 | Electrochemical sensor |
| CN102426181A (en) * | 2011-09-01 | 2012-04-25 | 聊城大学 | Application of electrochemical sensor with magnetic conductive porous material as carrier in detection |
-
2013
- 2013-09-18 CN CN2013104250622A patent/CN103439395A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101329296A (en) * | 2007-12-20 | 2008-12-24 | 复旦大学 | Glucolase electrode based on magnetic carbon nano-tube and preparation method thereof |
| CN101629931A (en) * | 2009-07-31 | 2010-01-20 | 江苏科技大学 | Anti-ascorbate sensor electrode and preparation method thereof |
| CN101986148A (en) * | 2010-10-18 | 2011-03-16 | 上海市七宝中学 | Electrochemical sensor |
| CN102426181A (en) * | 2011-09-01 | 2012-04-25 | 聊城大学 | Application of electrochemical sensor with magnetic conductive porous material as carrier in detection |
Non-Patent Citations (2)
| Title |
|---|
| 张玉珍: "几种贵金属纳米复合材料的制备、表征及电化学分析性能研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》, 15 September 2012 (2012-09-15) * |
| 熊志刚 等: "磁性纳米粒子固定葡萄糖氧化酶修饰电极电致化学发光葡萄糖传感器", 《分析化学》, 30 June 2010 (2010-06-30) * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111458390A (en) * | 2020-04-11 | 2020-07-28 | 石河子大学 | Fe3O4Preparation method and application of modified electrode material |
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Application publication date: 20131211 |