CN103884764A - Fast detector capable of detecting antibiotics and pesticide residue in milk simultaneously - Google Patents
Fast detector capable of detecting antibiotics and pesticide residue in milk simultaneously Download PDFInfo
- Publication number
- CN103884764A CN103884764A CN201410142301.8A CN201410142301A CN103884764A CN 103884764 A CN103884764 A CN 103884764A CN 201410142301 A CN201410142301 A CN 201410142301A CN 103884764 A CN103884764 A CN 103884764A
- Authority
- CN
- China
- Prior art keywords
- electrode
- impedance
- milk
- microcontroller
- array
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
Abstract
The invention discloses a fast detector capable of detecting antibiotics and pesticide residue in milk simultaneously, belonging to the technical field of security detection of agricultural products. The fast detector is composed of an array type immunosensor, an analog multi-way switch, a detection circuit, a microcontroller, a display screen, keys and a power supply. Various antibiotic antibodies are fixed on the surfaces of half of working electrodes of the array type immunosensor of the fast detector, and various pesticide antibodies are fixed on the surfaces of the other half of the electrodes, so that the detector can simultaneously detect antibiotics and pesticide residue in a milk sample simultaneously through one sampling; the fast detector has the characteristics of high detection efficiency, low detection cost, short detection time and the like, can detect ten kinds of antibiotics and five kinds of pesticide residue in milk simultaneously through one sampling, can reach the detection limit of 1 microgram/L, and is suitable for on-site rapid detection of milk.
Description
Technical field
The present invention relates to a kind of fast detector that can simultaneously detect Antibiotics and pesticide residues in milk, belong to agricultural product security detection technique field.
Technical background
In recent years, along with developing rapidly of China's livestock breeding industry, milk yield increases substantially, and fresh milk and dairy produce have become the important component part in the people (especially old man and children) life food.But the widespread use in Modern Animal Husbandry of microbiotic and agricultural chemicals, inevitably causes the problem that exceeds standard of Antibiotics and pesticide residues in milk.The main safety detection index of the microbiotic in milk and residues of pesticides Chang Zuowei milk.Strengthen the detection to Antibiotics and pesticide residues in milk, to ensureing that human health has very profound significance.
Traditional Antibiotics and pesticide residues detection method mainly contains: gas chromatography (GC), high performance liquid chromatography (HPLC), Chromatography/Mass Spectrometry coupling technique (GC/LC-MS), capillary electrophoresis (CE), fluorescence analysis, euzymelinked immunosorbent assay (ELISA) (ELISA).Although these method selectivity are good, highly sensitive, accuracy is high, detection limit is low, can detect multiple element or compound, but it needs expensive instrument and equipment, sample pretreatment process is loaded down with trivial details, time-consuming simultaneously, and the technical merit requirement to analyst is very high, is unsuitable for field quick detection.Compared with traditional analytical approach, immunosensor is that high-sensitive sensor technology is combined with antigen, antibody specific reaction, there is following features: the selectivity that (1) is higher, therefore do not need tested component to separate, need not carry out pre-service to sample.(2) simple in structure, volume is little, easy to use, and particularly portable immunosensor is very beneficial for the Fast Measurement of agricultural product security quality.(3) can realize continuous on-line detection, make the quality control of food processing process become easy.(4) fast response time, amount of samples is few, and compared with other large-sized analytic instruments, immunosensor cost of manufacture is low, and can Reusability.
At present detecting instrument safely and fast in milk product, conventionally can only detection of antibiotics or residues of pesticides.In view of antibiotic residue and the residues of pesticides serious phenomenon that exceeds standard.Especially need to detect the rapid detection apparatus of the Antibiotics and pesticide residues in milk simultaneously, like this can be in primary sample, detect simultaneously and in milk, whether contain Antibiotics and pesticide residues and whether exceed standard.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of fast detector that can simultaneously detect Antibiotics and pesticide residues in milk is provided, in the sampling of a sample, realize Antibiotics and pesticide residues in the milk information such as whether exceed standard simultaneously.Can be used for the safe fast-field evaluations of dairy products quality in site such as milk, and the related data of mensuration is uploaded to database at any time, be conducive to the construction of the quality of dairy products traceability systems such as milk.
The technical scheme that the present invention takes is as follows:
The fast detector that can simultaneously detect Antibiotics and pesticide residues in milk, is characterized in that, by array immunosensor, analog multichannel switch, testing circuit, microcontroller, display screen, button and electric power generating composition;
Described array immunosensor, formed by a circular electrode dish, centre bit is equipped with electrode and contrast electrode, periphery is equally distributed working electrode, in working electrode, half is fixed with different types of antibiotic antibody, second half is fixed with different types of pesticide antibody, electrode, contrast electrode are equated with the distance of each working electrode, peripheral and the middle hole that has equal diameters of circular electrode dish, can be by working electrode, contrast electrode with in electrode electrode insertion hole, each working electrode terminals access analog multichannel switch;
Described analog multichannel switch, the impedance signal successively array immunization sensor being produced respectively gathers and delivers to testing circuit;
Described testing circuit is made up of feed circuit, detection chip, toggle switch and demarcation resistance, and feed circuit are connected with detection chip with microcontroller, adopts first and obtains steady power voltage supply through the method for wave filter voltage stabilizing again through transformer pressure-reducing; Detection chip is connected with demarcation resistance by toggle switch, detection chip produces driving voltage and is applied on array immunization sensor and collects response signal under the control of microcontroller, after discrete Fourier transform (DFT), obtain real part and imaginary part, and output to microcontroller;
On described microcontroller, move trace routine, mould value by the impedance real part receiving and imaginary part by impedance and phase calculation formula calculate mould value and the phase angle of impedance, after calibration, obtaining real impedance values, with set react before resistance value compare, obtain rate of change and reach a conclusion with typical curve contrast, delivering to display screen and show;
Described display screen is connected with microcontroller, for showing data and the window as user interactive;
Described button is connected with testing circuit with microcontroller, is provided with startup, starts, resets, stops key and four sensing range gears, for inputting instruction and detected parameters;
Described power supply is connected with feed circuit.
Operating voltage between working electrode and the contrast electrode of described fast detector is 300mV.
The model of described display screen is LED12864.
In the microprocessor of described detector, insert the database of impedance rate of change and Antibiotics and pesticide residues concentration relationship.
In the detection milk of described fast detector, the step of the method for Antibiotics and pesticide residues is as follows:
1) open detector, array-type sensor is put into test end liquid and measure initial impedance value A
1, and preserve;
2) take out array-type sensor, after rinsing with ultrapure water, put into pretreatment sample liquid and hatch 10min;
3) take out array-type sensor, after rinsing with ultrapure water, put into test end liquid and measure resistance value A
2;
4) according to change in impedance value formula computing impedance value rate of change, and according to the concentration of inserting in advance impedance rate of change in database and microbiotic or residues of pesticides concentration relationship typical curve and calculate microbiotic or agricultural chemicals.
Step 2) described in the disposal route of pretreatment sample liquid be:
Milk sample is filtered by aseptic miillpore filter (0.20 micron) and use 5 times of PBS solution (0.1M, pH=7.5) dilutions, for subsequent use.
Described in step 4), change in impedance value formula is: rate of change=| A
1-A
2|/A
1.
The fast detector ultimate principle that can simultaneously detect Antibiotics and pesticide residues in milk provided by the present invention is: when the array immunosensor of fixing different microbiotic and pesticide antibody is inserted in sample liquid, if have corresponding microbiotic and agricultural chemicals in sample liquid, because forming immune complex, the immune response between antibody and antigen hinders electronics transfer between test end liquid and immunosensor, and then the variation that produces impedance signal, the impedance signal collection successively array immunization sensor being produced respectively by analog multichannel switch is sent in detector, and then in working sample liquid, whether there are certain microbiotic and an agricultural chemicals, and the information such as determine whether to exceed standard.
Beneficial effect of the present invention: detector of the present invention can be realized the detection that simultaneously completes microbiotic and agricultural chemicals in milk in the sample introduction of a sample.Save detection time like this, also reduced the consumption of reagent simultaneously, reduced testing cost.Make up in the current instrument for milk microbiotic and Pesticides Testing, prepared respectively sample, detected respectively microbiotic and agricultural chemicals in milk, can not detect the defect of microbiotic and agricultural chemicals in milk simultaneously.
Accompanying drawing explanation
Fig. 1 is a kind of fast detector structured flowchart that can simultaneously detect Antibiotics and pesticide residues in milk of the present invention.
Fig. 2 is disc type array immunization sensor electrode distribution plan.
Fig. 3 is feed circuit schematic diagram in the present invention.
Fig. 4 is testing circuit schematic diagram in the present invention.
Embodiment
Below in conjunction with drawings and Examples, technical scheme of the present invention is elaborated, but the present invention is not subject to the restriction of embodiment.
Fig. 1 is a kind of structured flowchart that can simultaneously detect the fast detector of Antibiotics and pesticide residues in milk of the present invention.Detector is made up of testing circuit, array immunosensor, analog multichannel switch, power supply, button, microcontroller and display screen.Wherein testing circuit is made up of feed circuit, detection chip, toggle switch, demarcation resistance.Testing circuit is used for producing driving voltage and is applied on array immunization sensor, with the line number word processing of going forward side by side of the response signal after post-sampling excitation, result is sent into microcontroller; Microcontroller and the trace routine of moving above thereof are processed again to input signal, and the operation of whole system is controlled and responded; Button is used for inputting instruction and detected parameters; Display screen is used for quantizing output and presents final testing result, is the interactive interface of user and system; Power supply is whole system power supply.
Fig. 2 is array immunosensor distribution of electrodes figure.Described array immunosensor is made up of a circular electrode disk, centre bit is equipped with electrode and contrast electrode, periphery is equally distributed working electrode, electrode, contrast electrode are equated with the distance of each working electrode guaranteeing, make each working electrode and the resistance value that having between electrode equated.Peripheral and the middle hole that has equal diameters of circular electrode disk, can be by working electrode, contrast electrode with in electrode electrode insertion hole.Three electrode workplace inserts test end liquid, each working electrode terminals access analog multichannel switch, and the impedance signal collection successively array immunization sensor being produced respectively by analog multichannel switch is sent in detector testing circuit.Contrast electrode and electrode is directly received in testing circuit.Fixing respectively antibiotic antibody and pesticide antibody with nanometer-material-modified good working electrode surface.Between working electrode and contrast electrode, add the operating voltage of 300 millivolts, what in test fluid, measure is working electrode and to the resistance value between electrode.If have the corresponding microbiotic of sessile antibody and agricultural chemicals in sample liquid, cause respective sensor in array immunization sensor to send signal, thereby determine and contain which kind of microbiotic in sample and agricultural chemicals has residual and whether exceeds standard.
Described array immunosensor, has fixed respectively metrifonate, Rogor, chlopyrifos, sevin, 5 kinds of pesticide antibodies of carbofuran and kanamycins, penicillin, cefalexin, neomycin, gentamicin, streptomysin, tetracycline, aureomycin, terramycin, 10 kinds of antibiotic antibodies of fortimicin on array working electrode.Before sessile antibody, working electrode surface is modified by nano material, then drip be coated with 2 μ L(concentration be 5 μ g/mL) antibody-solutions to electrode surface, after naturally drying prepared by array immunosensor.
The microcontroller of described detector is selected STC89C52, loads trace routine on it.Feed circuit in testing circuit form and principle as shown in Figure 3, by transformer T1, bridge rectifier circuit BR1, electrochemical capacitor C1, C3, common capacitor C 2, C4, three terminal regulator U1 formation, its effect is the Power supply for provide+5V of whole system.In the design, the effect of electrochemical capacitor C1, C2 is filtering, simply say while being exactly the rising of electric capacity both end voltage, and capacitor charging, when lower voltage, capacitor discharge, the gradient while allowing lower voltage becomes gently, thereby plays the effect of filtering.The effect of common capacitor C 2, C4 is to prevent self-excitation, and it can absorb high frequency energizing signal to keep stable, makes circuit there is no pumping signal, thereby prevents self-excitation.The effect of three terminal regulator U1 be by output voltage stabilization on+5V, connect respectively+5V of the output and ground of U1 and ground connection.
In described testing circuit, the formation of core testing circuit as shown in Figure 4: by detection chip U3, toggle switch SW3, demarcate resistance R 1, R2, R3, R4, R5, common capacitor C 7, C8 form, its effect is produce driving voltage and be applied on immunosensor, with the line number word processing of going forward side by side of the response signal after post-sampling excitation, result is sent into microcontroller.The effect of wherein demarcating resistance R 1, R2, R3 is as external feedback resistance.Toggle switch SW3 is 4-bit DIP switch, and its effect is to select the resistance of suitable demarcation to be connected into testing circuit to prevent that response signal from exceeding the range of detection chip and guaranteeing system linearity characteristic.The effect of demarcating resistance R 4, R5 is to be connected between 15,16 pins and power supply of detection chip as pull-up resistor.The effect of capacitor C 7, C8 is used for filtering and shielding, and prevents electromagnetic interference (EMI).Detection chip U3 is a high-precision impedance measurement chip, and inside is integrated with 12, and sampling rate is up to the frequency generator of the AD converter of 1MSPS.Its effect is that the driving voltage that produces characteristic frequency encourages element under test, the response signal obtaining is sampled by ADC, and carry out discrete Fourier transform by the DSP on sheet, after Fourier transform, return to the value of real part and the imaginary values that under this output frequency, obtain, and result is sent into microcontroller.15,16 pins are connected with+5V power supply by pull-up resistor R4, R5,12,13,14 pin earths, 9,10,11 pin parallel connections are connected with+5V power supply, 4, between 5 pins by toggle switch with demarcate resistance and be connected, 5,6 be used for connecing element under test.
Fast detector provided by the present invention, concrete use procedure is as follows: use nano material to carry out chemical modification array-type sensor working electrode surface before use, improve the sensitivity that sensor detects, fix respectively different types of microbiotic and pesticide antibody at array immunosensor working electrode surface afterwards.Then array immunosensor is put into refrigerator, under 4 ° of C, save backup.When use, open the power switch of detector, array-type sensor is put into test end liquid and measure initial impedance value A1, and preserve.Immunosensor is put into the sample liquid of handling well in advance and hatch 10 minutes, then sensor is connected to detector carries out impedance measurement, obtain the resistance value A2 measuring for the second time, microcontroller is delivered to display screen and is shown.Calculate rate of change, rate of change computing formula is as follows:
Rate of change=| A1-A2|/A1
If contain microbiotic or agricultural chemicals in sample liquid,, containing relevant work electrode generation specific immune response, cause reacted respective sensor resistance value obviously to increase.The difference of A1 and A2 is larger, shows to detect the concentration that contains certain microbiotic or residues of pesticides in solution higher.Contrast standard curve obtains the concentration of microbiotic in sample or residues of pesticides, shows at display screen.Impedance rate of change and Antibiotics and pesticide residues concentration relationship typical curve in storer, are inserted, according to the size of each sensor impedance rate of change, can show at the display screen of instrument the concentration information that contains which kind of microbiotic, agricultural chemicals and Antibiotics and pesticide residues in the sample of detection.
Fast detector method of operating provided by the present invention is simple, detection time is shorter, can in primary sample, realize the qualitative, quantitative of the Antibiotics and pesticide residues in milk measures, there is detection time short, highly sensitive, good stability, high repeatability and other advantages, meet China to microbiotic Fast Determination of Pesticide Residue technical development in milk and internationalization requirement.
Claims (7)
1. the fast detector that can simultaneously detect milk Pesticides and antibiotic residue, is characterized in that, by array immunosensor, analog multichannel switch, testing circuit, microcontroller, display screen, button and electric power generating composition;
Described array immunosensor, formed by a circular electrode dish, centre bit is equipped with electrode and contrast electrode, periphery is equally distributed working electrode, in working electrode, half is fixed with different types of antibiotic antibody, second half is fixed with different types of pesticide antibody, electrode, contrast electrode are equated with the distance of each working electrode, peripheral and the middle hole that has equal diameters of circular electrode dish, can be by working electrode, contrast electrode with in electrode electrode insertion hole, each working electrode terminals access analog multichannel switch;
Described analog multichannel switch, the impedance signal successively array immunization sensor being produced respectively gathers and delivers to testing circuit;
Described testing circuit is made up of feed circuit, detection chip, toggle switch and demarcation resistance, and feed circuit are connected with detection chip with microcontroller, adopts first and obtains steady power voltage supply through the method for wave filter voltage stabilizing again through transformer pressure-reducing; Detection chip is connected with demarcation resistance by toggle switch, detection chip produces driving voltage and is applied on array immunization sensor and collects response signal under the control of microcontroller, after discrete Fourier transform (DFT), obtain real part and imaginary part, and output to microcontroller;
On described microcontroller, move trace routine, mould value by the impedance real part receiving and imaginary part by impedance and phase calculation formula calculate mould value and the phase angle of impedance, after calibration, obtaining real impedance values, with set react before resistance value compare, obtain rate of change and reach a conclusion with typical curve contrast, delivering to display screen and show;
Described display screen is connected with microcontroller, for showing data and the window as user interactive;
Described button is connected with testing circuit with microcontroller, is provided with startup, starts, resets, stops key and four sensing range gears, for inputting instruction and detected parameters;
Described power supply is connected with feed circuit.
2. fast detector described in claim 1, is characterized in that, the operating voltage between working electrode and contrast electrode is 300mV.
3. fast detector described in claim 1, is characterized in that, the model of described display screen is LED12864.
4. fast detector described in claim 1, is characterized in that, the microprocessor in the built-in detection chip of described detector has been inserted the database of impedance rate of change and Antibiotics and pesticide residues concentration relationship.
5. a method for Antibiotics and pesticide residues in the detection milk of fast detector described in claim 1, is characterized in that, step is as follows:
Open detector, array-type sensor is put into test end liquid and measure initial impedance value A
1, and preserve;
Take out array-type sensor, after rinsing with ultrapure water, put into pretreatment sample liquid and hatch 10min;
Take out array-type sensor, after rinsing with ultrapure water, put into test end liquid and measure resistance value A
2;
According to change in impedance value formula computing impedance value rate of change, and according to the concentration of inserting in advance impedance rate of change in database and microbiotic or residues of pesticides concentration relationship typical curve and calculate microbiotic or agricultural chemicals.
6. method described in claim 5, it is characterized in that, step 2) described in the disposal route of pretreatment sample liquid be: milk sample is filtered by aseptic miillpore filter (0.20 micron) and uses PBS solution (0.1M, pH=7.5) to dilute 5 times, for subsequent use.
7. method described in claim 5, is characterized in that, change in impedance value formula is described in step 4): rate of change=| A
1-A
2|/A
1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410142301.8A CN103884764A (en) | 2014-04-10 | 2014-04-10 | Fast detector capable of detecting antibiotics and pesticide residue in milk simultaneously |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410142301.8A CN103884764A (en) | 2014-04-10 | 2014-04-10 | Fast detector capable of detecting antibiotics and pesticide residue in milk simultaneously |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103884764A true CN103884764A (en) | 2014-06-25 |
Family
ID=50953776
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410142301.8A Pending CN103884764A (en) | 2014-04-10 | 2014-04-10 | Fast detector capable of detecting antibiotics and pesticide residue in milk simultaneously |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103884764A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104535729A (en) * | 2014-12-23 | 2015-04-22 | 温岭市太平高级职业中学 | Portable antibiotic detection pocket |
| CN104965081B (en) * | 2015-05-29 | 2016-08-17 | 刘晓竹 | Antibody antigen detection method based on mobile device |
| CN108061704A (en) * | 2017-12-06 | 2018-05-22 | 中国石油大学(华东) | A kind of single electrode crossed array wire beam electrode system corroded under Test coverage object |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103499686A (en) * | 2013-10-18 | 2014-01-08 | 山东理工大学 | Immunosensor-based resistance-type pesticide residue detector |
| CN103558257A (en) * | 2013-11-19 | 2014-02-05 | 山东理工大学 | Pesticide multiresidue detector based on array sensors |
| CN103558258A (en) * | 2013-11-19 | 2014-02-05 | 山东理工大学 | Antibiotic multiresidue detector based on array sensors |
-
2014
- 2014-04-10 CN CN201410142301.8A patent/CN103884764A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103499686A (en) * | 2013-10-18 | 2014-01-08 | 山东理工大学 | Immunosensor-based resistance-type pesticide residue detector |
| CN103558257A (en) * | 2013-11-19 | 2014-02-05 | 山东理工大学 | Pesticide multiresidue detector based on array sensors |
| CN103558258A (en) * | 2013-11-19 | 2014-02-05 | 山东理工大学 | Antibiotic multiresidue detector based on array sensors |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104535729A (en) * | 2014-12-23 | 2015-04-22 | 温岭市太平高级职业中学 | Portable antibiotic detection pocket |
| CN104965081B (en) * | 2015-05-29 | 2016-08-17 | 刘晓竹 | Antibody antigen detection method based on mobile device |
| CN108061704A (en) * | 2017-12-06 | 2018-05-22 | 中国石油大学(华东) | A kind of single electrode crossed array wire beam electrode system corroded under Test coverage object |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Krska et al. | Mycotoxin analysis: An update | |
| CN103940854A (en) | Rapid detector capable of simultaneously detecting pesticide and heavy metal residues in fruits and vegetables | |
| CN103558257B (en) | Pesticide multiresidue detector based on array sensors | |
| Cigić et al. | An overview of conventional and emerging analytical methods for the determination of mycotoxins | |
| CN103558258B (en) | Antibiotic multiresidue detector based on array sensors | |
| Ansari et al. | A portable lab‐on‐a‐chip instrument based on MCE with dual top–bottom capacitive coupled contactless conductivity detector in replaceable cell cartridge | |
| CN103940987A (en) | Rapid detector for simultaneously detecting aflatoxin and pesticides in peanuts | |
| CN103884764A (en) | Fast detector capable of detecting antibiotics and pesticide residue in milk simultaneously | |
| CN108776160B (en) | Method that is a kind of while detecting bisphenol-A and bisphenol S | |
| Bose et al. | Perfomance study of urease-PMMA-based aqueous urea sensor | |
| CN203759254U (en) | Flat source box for efficiency calibration of gram-scale solid powder sample | |
| Kestranek et al. | Chemiluminescent nitrogen detection (CLND) to measure kinetic aqueous solubility | |
| US9304096B2 (en) | Method of measuring a capacitance | |
| Chavanne et al. | Autonomous sensors for measuring continuously the moisture and salinity of a porous medium | |
| CN205506786U (en) | Gas sensor's demarcation frock | |
| CN103499686A (en) | Immunosensor-based resistance-type pesticide residue detector | |
| CN103308507A (en) | Analysis method for rapidly measuring free isocyanate (NCO) in polyurethane | |
| CN105911296A (en) | IV-type collagen chemiluminescence immunoassay kit and preparation method thereof | |
| CN101216423A (en) | Dairy food antibiotic race detection method based on surface plasma resonance | |
| CN103940865B (en) | A kind of belt-lactam antibiotics residues fast detector | |
| CN110780002A (en) | High-efficiency low-cost detection method for quantifying essential oil components | |
| EP1488230B1 (en) | Drift compensated magnetic permeability detector | |
| CN208013153U (en) | The cloud self-measuring instrument of chromatography instrument | |
| CN201514377U (en) | Incubation module of chemiluminescent measurement instrument | |
| Bonzon et al. | Micropipette calibration by differential pressure measurements |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20140625 |
|
| RJ01 | Rejection of invention patent application after publication |