CN103018238B - Method for measuring iodide ions quickly and efficiently - Google Patents
Method for measuring iodide ions quickly and efficiently Download PDFInfo
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- CN103018238B CN103018238B CN201210527677.1A CN201210527677A CN103018238B CN 103018238 B CN103018238 B CN 103018238B CN 201210527677 A CN201210527677 A CN 201210527677A CN 103018238 B CN103018238 B CN 103018238B
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Abstract
The invention provides a method for measuring iodide ions quickly and efficiently. Metal nano-composite material (gold or silver) with good water-solubility and high molar absorptivity is taken as a probe, and a novel iodine ion sensor is formed under the action of restraining of iodine ions to oxidation aggregate of nano-composite material. The method can be successfully applied to measurement of iodine ions, and the lowest concentration of iodine ions, which can be detected through a visual method, can be 1nM; and compared with the traditional iodine ion measuring methods (such as a spectral method and a electrochemistry method) reported at present, the method provided by the invention has the advantage that the lowest concentration (1nM) is at least 1 order of magnitude lower than the detection limit obtained through the traditional method. The novel anti-aggregating type nano-composite material probe obtained in the invention can effectively avoid aggregate caused by other factors in a solution, and can improve the selectivity in measuring. Therefore, the method has the advantages of simplicity, quickness, high sensitivity and good selectivity, and can be applied to measurement of iodine ions in dairy salt and urine.
Description
Technical field:
The present invention relates to analysis detection field, particularly relate to the metal nano material of water-soluble, high absorptivity as the application of colourimetry probe in quick, highly sensitive detection iodide ion.
Background technology:
Iodide ion is prevalent in the ecosystem, for nerve grow and the metabolism of biosome plays vital effect [G.Aumont and J.C.Tressol, Analyst, 1986,3,841-843; M.Haldimann, B.Zimmerli, C.Als and H.Gerber, Clin.Chem., 1998,44,817-824; F.Jalali, M.J.Rajabi, G. Bahrami and M.Shamsipur, Anal.Sci., 2005,21,1533-1535].Such as, lack iodine and can cause spontaneous abortion, infant mortality raises, mental deficiency [L.Rong and T.Takeuchi, J. Chromatogr.A, 2004,1042,131-135; J.Jakmunee and K.Grudpan, Anal.Chim.Acta, 2001,438,299-304; F.Delange, B.Benoist, E.Pretell and J.T.Dunn, Thyroid, 2001,11,437-447].The World Health Organization (WHO) issues a statement, in the world the shortage of iodine be cause the topmost reason of mental deficiency [
http:// www.iccidd.org].Therefore, iodide ion is detected significant and urgent.But as everyone knows, halogen comprises fluorine, chlorine, bromine, iodine.They have similar physical property.And iodide ion has larger ionic radius, lower electric density and hydrogen bond Forming ability.These characteristics add difficulty [Z.Rodriguez-Docampo, S.I.Pascu, S.Kubik and S.Otto, J. Am.Chem.Soc., 2006,128, the 11206-11210 of selective determination iodide ion greatly; M.Vetrichelvan, R.Nagarajan and S.Valiyaveettil, Macromolecules, 2006,39,8303-8310; N.Narinder Singh and D.O.Jang, Org.Lett., 2007,9,1991-1994; S.Kubik, Chem.Soc.Rev., 2010,39,3648-3663].The assay method of current report has spectroscopic methodology [M.P. Arena, M.D.Porter and J.S.Fritz, Anal.Chem., 2002,74,185-190; A.K.Mahapatra, G. Hazra, J.Roy and P. Sahoo, J. Lumin., 2011,131,1255-1259; Z.B.Shang, Y. Wang and W.J.Jin, Talanta, 2009,78,364-369; M.Zhangand B.C.Ye, Chem.Commun., 2012,48,3647-3649; X.J.Wang, C.H.Zhang, L.H.Feng and L.W.Zhang, Sens.Actuators, B, 2011,156,463-466; Y.M.Chen, T.L.Cheng and W.L.Tseng, Analyst, 2009,134,2106-2112; P. Pienpinijtham, X.X.Han, S.Ekgasit and Y. Ozaki, Anal.Chem., 2011,83,3655-3662], electrochemical process [D.Phokharatkul, C.Karuwan, T.Lomas, D.Nacapricha, A.Wisitsoraat and A.Tuantranont, Talanta, 2011,84,1390-1395; L.Vitali, B.L.Horst, M.Heller, V.T.F á vere and G. A.Micke, J. Chromatogr.A, 2011,1218,4586-4591; H.Ciftci and U.Tamer, Anal.Chim.Acta, 2011,687,137-140].In spectroscopic methodology field, super molecular compound is mostly adopted to measure iodide ion [A.Kumar, R.K.Chhatra and P.S.Pandey, Org.Lett., 2010,12,24-27; H.H.Wang, L.Xue and H.Jiang, Org.Lett., 2011,13,3844-3847; M.A.Tetilla, M.Carla Aragoni, M.Arca, C.Caltagirone, C.Bazzicalupi, A.Bencini, A.Garau, F.Isaia, A.Laguna, V. Lippolis and V.Meli, Chem.Commun., 2011,47,3805-3807].Although these sensors have good selectivity, also there are some defects, as synthesis super molecular compound relates to comparatively complicated organic synthesis step, the cost of agents useful for same is higher; And super molecular compound is often water insoluble, be difficult to directly measure iodide ion in water; The detectability measuring iodide ion with super molecular compound is often higher.Therefore, setting up novel, efficient iodide ion sensor will be a challenge.
Colourimetry is visible owing to having naked eyes, and easily observation and the advantage do not needed by advanced instrument, be more and more used to identification and detection [J.Liu and Y.Lu, J.Am.Chem.Soc., 2005,127, the 12677-12683 of determinand; C.J.Murphy, A.M.Gole, J.W.Stone, P.N.Sisco, A.M.Alkilany, E.C.Goldsmith and S.C.Baxter, Acc.Chem.Res., 2008,41,1721-1730; Y. Tan, X.Su, E.Liu and J.S.Thomsen, Anal.Chem., 2010,82,2759-2765; N.Nath and A.Chilkoti, Anal.Chem., 2002,74,504-509].But compared with supermolecule sensor, the report that metal nano material sensor is used for iodide ion mensuration is considerably less.One section of document is only had to be report metal nano material colorimetric method for determining iodide ion at present.Its measuring principle utilizes iodide ion to atom restructuring effect [J.Zhang, X.W.Xu, C.Yang, F.Yang and X.R.Yang, Anal.Chem., 2011,83,3911-3917] of CuAu core/shell nanometer material.The present invention utilizes the resistant to aggregation effect of iodide ion to metal nano material to establish the new method of testing of iodide ion.Adopt resistant to aggregation principle to measure the interference of the nano material congregation can effectively avoiding other factors in solution to cause, the selectivity of mensuration improves greatly.The method can successfully realize iodide ion quick, efficiently measure, the mensuration of common negative ion to iodide ion is not almost disturbed.The method is expected to the mensuration being used as iodide ion in salt and urine.
Summary of the invention:
The object of this invention is to provide a kind of assay method of iodide ion fast and efficiently; Especially provide nano material as the novelty teabag of colourimetry probe in iodide ion mensuration.
An object of the present invention realizes by following technical measures:
A, under the existence of dressing agent, by phenolic compound as the solution of reductive agent reducing metal ionically-soluble salt (silver nitrate, chlorine gold (III) acid) to prepare functional silver/gold nano-material;
B, the metal nano material getting certain volume add the buffer solution with certain pH of certain volume, and certain density iodide ion standard solution to be measured, subsequently, adds the certain density reagent that metal nano material can be made to assemble, and develop the color 5 minutes under room temperature.
Object of the present invention also realizes by following technical measures:
The dressing agent of described metal nano material, is selected from lauryl sodium sulfate, sodium polyphosphate, cetyl trimethyl ammonium bromide, PDDA polymkeric substance, PSS polymkeric substance, trisodium citrate; Phenols reductive agent used is phenol, catechol, dopamine, p-dihydroxy-benzene, gallic acid; The described pH scope with the buffer solution of certain pH is 2.0-9.0; Measuring buffer solution used is hac buffer, citric acid solution, carbonate buffer solution, phosphate buffer solution, Tris buffer solution; The described reagent that metal nano material can be made to assemble is hydrogen peroxide, potassium permanganate, potassium dichromate, sodium hypochlorite, ammonium peroxydisulfate, and the concentration of the reagent that metal nano material can be made to assemble used is 2 × 10
-4-5 × 10
-2mol/L.
The interference that the metal nano material that " resistant to aggregation " type nano-probe involved in the present invention can effectively avoid other factors in solution to cause is assembled, selectivity improves greatly.The method minute only needs 5 minutes, and agents useful for same is simple, cheap, and cost is lower.
Accompanying drawing illustrates:
Fig. 1 is that the color after the AgNPs of the sodium polyphosphate modification of invention preparation adds variable concentrations iodide ion and hydrogen peroxide changes.
Fig. 2 is that the absorption spectrum after the AgNPs of the trisodium citrate modification of invention preparation adds variable concentrations iodide ion and hydrogen peroxide changes.
Fig. 3 is the graph of a relation that the absorbance of the AgNPs that the PSS of invention preparation modifies changes with iodide ion concentration.
Fig. 4 is that the AgNPs of the trisodium citrate modification of invention preparation is to the absorption spectrum response diagram of other negative ion.
Embodiment:
Embodiment 1:
A, in the 50mL liquor argenti nitratis ophthalmicus being dissolved with 0.1mM, add the sodium polyphosphate of 5mL0.01M as coating material, the 50mL catechol solution of 0.2mM is joined in above-mentioned mixed liquor, back flow reaction 1h, obtains the water-soluble silver nano material that sodium polyphosphate is modified;
B, get 2mL Nano Silver and add 0.1mL, the hac buffer of 0.1M (pH 2.2), certain density iodide ion standard solution to be measured, subsequently, after adding 10 μ L 30% aqueous hydrogen peroxide solutions, chromogenic reaction 5 minutes.
Embodiment 2:
A, in the 25mL liquor argenti nitratis ophthalmicus being dissolved with 0.1mM, add the trisodium citrate of 1mL 0.01M as coating material, the Dopamine hydrochloride of the 10mL of 0.2mM is joined in above-mentioned mixed liquor, react 8h under normal temperature, obtain the water-soluble silver nano material that trisodium citrate is modified;
B, get the hac buffer that 2mL Nano Silver adds 0.1mL 0.1M (pH 4.0), certain density iodide ion standard solution to be measured, subsequently, after adding 1mL0.2mM liquor potassic permanganate, chromogenic reaction 5 minutes.
Embodiment 3:
A, in the 50mL chlorauric acid solution being dissolved with 0.1mM, add the lauryl sodium sulfate of 5mL 0.01M as coating material, the phenol solution of the 20mL of 0.2mM is joined in above-mentioned mixed liquor, the sodium hydroxide solution adding 0.1M regulates the pH of mixed liquor to be 8.0, react 24h under normal temperature, obtain the water-soluble gold nano material that lauryl sodium sulfate is modified;
B, get 2mL nm of gold and add 0.1mL, the citric acid solution of 0.1M (pH 9.0), certain density iodide ion standard solution to be measured, subsequently, after adding the superoxol of 1mL 0.2mM, chromogenic reaction 5 minutes.
Claims (4)
1. quick, the efficient detection method of iodide ion, is characterized in that:
A, be selected from lauryl sodium sulfate, sodium polyphosphate, cetyl trimethyl ammonium bromide, PDDA polymkeric substance, a kind of as under the condition of dressing agent in PSS polymkeric substance, by taking from one in phenol, catechol, dopamine, the gallic acid solution as reductive agent reduction silver nitrate or chlorine gold (III) acid to prepare functional silver/gold nano-material;
B, the metal nano material getting the above-mentioned preparation of certain volume add the buffer solution with certain pH of certain volume, certain density iodide ion standard solution to be measured, subsequently, adding the certain density a kind of reagent as making nano material assemble taken from hydrogen peroxide, potassium permanganate, potassium dichromate, sodium hypochlorite, ammonium peroxydisulfate, developing the color 5 minutes under room temperature.
2. quick, the efficient detection method of iodide ion according to claim 1, is characterized in that the described pH scope with the buffer solution of certain pH is 2.0-9.0.
3. quick, the efficient detection method of iodide ion according to claim 1, is characterized in that the described buffer solution with certain pH is hac buffer, citric acid solution, carbonate buffer solution, phosphate buffer solution, Tris buffer solution.
4. quick, the efficient detection method of iodide ion according to claim 1, is characterized in that the described concentration adding the certain density a kind of reagent as making nano material assemble taken from hydrogen peroxide, potassium permanganate, potassium dichromate, sodium hypochlorite, ammonium peroxydisulfate is 2 × 10
-4-5 × 10
-2mol/L.
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CN104020164A (en) * | 2014-06-06 | 2014-09-03 | 重庆大学 | Method for detecting content of trace iodine ions in chlorin-alkali brine and industrial salt |
CN104111309B (en) * | 2014-06-23 | 2015-12-09 | 神马实业股份有限公司 | The method for rapidly testing of iodide ion content in nylon polymer |
CN106404766A (en) * | 2016-08-30 | 2017-02-15 | 中南林业科技大学 | Preparation method of nanogold colorimetric probe and method for detecting iodide ions by using nanogold colorimetric probe |
HU231183B1 (en) * | 2018-06-15 | 2021-07-28 | Ioi Auranae Kft. | Process and kit for quick and inexpensive detection of iodide ions in aqueous solutions |
CN113340888B (en) * | 2021-07-02 | 2023-11-21 | 长沙塞克陆德医疗科技有限公司 | Reagent, kit and detection method for quantitative detection of blood iodine |
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US20050147963A1 (en) * | 2003-12-29 | 2005-07-07 | Intel Corporation | Composite organic-inorganic nanoparticles and methods for use thereof |
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CN1821752A (en) * | 2006-03-30 | 2006-08-23 | 湖南大学 | Nano sensor for detecting phenolic substance and its detecting method |
CN102221529A (en) * | 2011-03-31 | 2011-10-19 | 吉林大学 | Method for rapidly detecting residuals of organophosphorus pesticides in vegetables by utilizing Au nano-particle colorimetric method |
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