CN103293202B - Method for rapidly detecting forchlorfenuron residue in fruit juice - Google Patents

Method for rapidly detecting forchlorfenuron residue in fruit juice Download PDF

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Publication number
CN103293202B
CN103293202B CN201310216460.3A CN201310216460A CN103293202B CN 103293202 B CN103293202 B CN 103293202B CN 201310216460 A CN201310216460 A CN 201310216460A CN 103293202 B CN103293202 B CN 103293202B
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China
Prior art keywords
electrode
cppu
electrolytic cell
fruit juice
forchlorfenuron
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Expired - Fee Related
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CN201310216460.3A
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Chinese (zh)
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CN103293202A (en
Inventor
徐琴
蔡丽娟
胡效亚
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Yangzhou University
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Yangzhou University
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Publication of CN103293202A publication Critical patent/CN103293202A/en
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Abstract

The invention relates to a method for rapidly detecting forchlorfenuron residue in fruit juice. According to the technical scheme of the invention, the method comprises the steps of: adding a phosphate buffered solution into an electrolytic cell, adding a forchlorfenuron solution into the electrolytic cell, starting a magnetic stirrer, setting constant potential and enrichment time of electrode pretreatment, after the enrichment is completed, putting a working electrode, a reference electrode and an auxiliary electrode into the electrolytic cell containing 10ml of phosphate buffered solution, and measuring peak current signals. The method can be used for overcoming the defects that in the prior art, the emulsification phenomenon is easy to generate, the steps of purification treatment are relatively complicated, the purification effect is not ideal, the requirements for instruments and equipment are high and the like. According to the method, the sample treatment is easy and feasible, the instruments are stable in performance, and the results are reliable and can be directly displayed without needing professionals; the consumed time is short, the detection cost is low, the degree of automation is high, the operation is easy and convenient, the sampling amount is small, the method is especially applicable to the detection of forchlorfenuron content in plants, and juice original samples can be directly taken for analysis without a complex pretreatment process.

Description

A kind of method that in quick detection fruit juice, CPPU is residual
Technical field
The present invention relates to a kind of based on electrochemical method, a kind of method that particularly in quick detection fruit juice, CPPU is residual.
Background technology
In recent years, CPPU, as a kind of exogenous hormone, is applied to the production of melon and fruit more and more widely, is brought huge economic benefit to numerous orchard workers and enterprise.But it also brings stern challenge and threat to agricultural product security simultaneously.
Before making the present invention, the existing residual quantity adopting CPPU in Watermelon by HPLC, grape and Kiwi berry.There is employing liquid-liquid extraction-high performance liquid chromatography.But the method organic reagent use amount is large, and easily produces emulsion in leaching process, and purified treatment step is relatively loaded down with trivial details.Also someone adopts tablets by HPLC-MS to remain CPPU to detect, and pre-treatment adopts anionite propyl group ethylenediamine to carry out purified treatment to matrix, but clean-up effect is undesirable, and the method requires higher to instrument and equipment.
Summary of the invention
Object of the present invention is just to overcome above-mentioned defect, develops the device based on electrochemical method determining CPPU.
Technical scheme of the present invention is:
The method that in quick detection fruit juice, CPPU is residual, its major technique step is:
(1) phosphate buffered solution is joined in electrolytic cell;
(2) CPPU solution is added in this electrolytic cell;
(3) magnetic stirring apparatus is started;
(4) the pretreated constant potential of electrode, enrichment time are set;
(5), after enrichment terminates, working electrode, contrast electrode, auxiliary electrode are put into the electrolytic cell containing 10ml phosphate buffered solution;
(6) peak current signal is measured.
Described working electrode is carbon electrode, and described contrast electrode is saturated potassium chloride electrode, and described auxiliary electrode is platinum electrode.
Described working electrode is located on megohmite insulant, and a circle porous mass is located at the outer ring of insulating matter.
Described carbon electrode diameter is adjustable.
Advantage of the present invention and effect are sample preparation simple possible, dissolve with ethanol; Instrument performance is stablized, reliable results, and easy and simple to handle, automaticity is high, and result directly shows, and does not need professional; Consuming time short, 3min can obtain analysis result, and testing cost is low, automaticity is high, easy and simple to handle and sampling amount is little, is particularly useful for the detection of CPPU content in plant, can directly take fruit juice former state to analyze, without the need to the pretreatment process of complexity.
Other concrete advantages of the present invention and effect will go on to say below.
Embodiment
CPPU solution is joined in PBS, constant potential and enrichment time are set, make CPPU be enriched to carbon electrodes, in blank PBS, then measure the current signal of CPPU.The content of CPPU is proportional to the current signal strength of output, and the instrument made is self-reacting device, and one-shot measurement about 3min consuming time, reagent dosage can control at 10 μ l.Especially working electrode, contrast electrode and auxiliary electrode are made in three-electrode system immersion electrolytic cell and detect, thus both ensured CPPU in sample by abundant enrichment, ensure again few sample size, like this when carrying out CPPU and detecting with less sample, thus also ensure not pollute environment.
Electrolytic solution is neutral electrolyte, after being added by CPPU solution, can direct apparatus of the present invention measure.Neutral phosphate buffered saline(PBS) selected by electrolytic solution.
Based on the measurement mechanism of electrochemical method determining CPPU character, comprise electrochemical workstation, electrolytic cell, working electrode, contrast electrode and auxiliary electrode to form, working electrode, contrast electrode and auxiliary electrode is it is characterized in that to make three-electrode system, working electrode is carbon electrode, electrode size can be adjusted as required, guarantee insert less electrolytic cell or carry out on-line checkingi with this, contrast electrode is saturated potassium chloride electrode, and auxiliary electrode is platinum electrode.Contrast electrode is placed in internal-filling liquid, and internal-filling liquid is conventional saturated potassium chloride solution etc.
During measurement, constant potential and enrichment time are first set, make CPPU be enriched to bare electrode surface, in blank PBS, then measure the current signal of CPPU.Monitoring lower-cut can be low to moderate 10 -14mol/L.The size of CPPU concentration is relevant with the current signal strength of output, thus by arranging of instrument itself, result is calculated display (automatically being completed by instrument).
Get 10 μ l CPPU solution and be placed in the electrolytic cell that 10ml PBS (phosphate buffered solution) is housed.
Three electrode new systems are all immersed in electrolytic solution.Open magnetic stirring apparatus, the pretreated current potential of electrode in electrochemical workstation and enrichment time are set, CPPU is made to be enriched to carbon electrodes, the electrolytic cell only containing 10ml PBS solution is put into after three-electrode system distilled water flushing is clean after enrichment terminates, press measurement switch to start to measure, can obtain the peak current signal that CPPU is corresponding after 3min, unit is A.Measure and terminate.
Electrochemical workstation comprises Survey Software and three electrode interfaces, and interface connects different electrodes respectively, and green connection working electrode, white connects contrast electrode, and redness connects auxiliary electrode.Neutral PBS solution selected by electrolytic solution.
In measurement mechanism of the present invention, the three-electrode system that working electrode, contrast electrode and auxiliary electrode are formed is inserted in electrolytic cell.Electrolytic cell adopts glass, and working electrode is located on megohmite insulant; Contrast electrode is placed in internal-filling liquid, and internal-filling liquid is conventional saturated potassium chloride solution, ensures to conduct electricity between electrode internal-filling liquid and external solution and internal-filling liquid does not ooze out; When working electrode diameter is large, need more sample and larger electrolytic cell, but the present invention can adopt the carbon electrode of different area as required, available less reagent, as reagent dosage can control at 10 μ l.Described reagent is the consumption that CPPU is measured at every turn.

Claims (4)

1. detect the method that in fruit juice, CPPU is residual fast, its step is:
(1) phosphate buffered solution is joined in electrolytic cell;
(2) CPPU solution is added in this electrolytic cell;
(3) magnetic stirring apparatus is started;
(4) the pretreated constant potential of electrode, enrichment time are set;
(5), after enrichment terminates, working electrode, contrast electrode, auxiliary electrode are put into the electrolytic cell containing 10ml phosphate buffered solution, working electrode is carbon electrode, and contrast electrode is saturated potassium chloride electrode, and auxiliary electrode is platinum electrode;
(6) peak current signal is measured.
2. the method that in a kind of quick detection fruit juice according to claim 1, CPPU is residual, it is characterized in that described working electrode is carbon electrode, described contrast electrode is saturated potassium chloride electrode, and described auxiliary electrode is platinum electrode.
3. the method that in a kind of quick detection fruit juice according to claim 1, CPPU is residual, is characterized in that working electrode is located on megohmite insulant, and a circle porous mass is located at the outer ring of insulating matter.
4. the method that in a kind of quick detection fruit juice according to claim 2, CPPU is residual, is characterized in that carbon electrode can freely control.
CN201310216460.3A 2013-05-29 2013-05-29 Method for rapidly detecting forchlorfenuron residue in fruit juice Expired - Fee Related CN103293202B (en)

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CN201310216460.3A CN103293202B (en) 2013-05-29 2013-05-29 Method for rapidly detecting forchlorfenuron residue in fruit juice

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CN103293202B true CN103293202B (en) 2015-06-17

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Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107619440A (en) * 2017-08-10 2018-01-23 南昌大学 A kind of CPPU artificial antigen and preparation method and the application of polyclonal antibody

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1560628A (en) * 2004-02-23 2005-01-05 南京大学 High-efficient liquid phase chromatographic analysing method for regulating pyrurine and its impurity
CN202066859U (en) * 2011-05-23 2011-12-07 无锡安迪生物工程有限公司 Rapid forchlorfenuron detection card

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1560628A (en) * 2004-02-23 2005-01-05 南京大学 High-efficient liquid phase chromatographic analysing method for regulating pyrurine and its impurity
CN202066859U (en) * 2011-05-23 2011-12-07 无锡安迪生物工程有限公司 Rapid forchlorfenuron detection card

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
"Development and validation of a direct competitive monoclonal antibody-based immunoassay for the sensitive and selective analysis of the phytoregulator forchlorfenuron";Celia Suárez-Pantaleón et al;《Anal Bioanal Chem》;20120419;第2019-2026页 *
"氯吡脲残留检测技术进展及趋势";雷绍荣等;《中国测试》;20111130;第37卷(第6期);第53-56页 *

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