CN202471663U - Pretreatment reagent kit for measuring thimerosal residues in animal derived food - Google Patents
Pretreatment reagent kit for measuring thimerosal residues in animal derived food Download PDFInfo
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- CN202471663U CN202471663U CN2011204468258U CN201120446825U CN202471663U CN 202471663 U CN202471663 U CN 202471663U CN 2011204468258 U CN2011204468258 U CN 2011204468258U CN 201120446825 U CN201120446825 U CN 201120446825U CN 202471663 U CN202471663 U CN 202471663U
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- Prior art keywords
- thimerosal
- centrifuge tube
- animal derived
- reagent kit
- pretreatment reagent
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- RTKIYNMVFMVABJ-UHFFFAOYSA-L thimerosal Chemical group [Na+].CC[Hg]SC1=CC=CC=C1C([O-])=O RTKIYNMVFMVABJ-UHFFFAOYSA-L 0.000 title claims abstract description 73
- 241001465754 Metazoa Species 0.000 title claims abstract description 46
- 235000013305 food Nutrition 0.000 title claims abstract description 46
- 239000003153 chemical reaction reagent Substances 0.000 title claims abstract description 37
- 229940033663 thimerosal Drugs 0.000 claims abstract description 65
- 238000000605 extraction Methods 0.000 claims abstract description 55
- 238000001914 filtration Methods 0.000 claims abstract description 17
- 239000012528 membrane Substances 0.000 claims abstract description 10
- 239000004743 Polypropylene Substances 0.000 claims abstract description 8
- -1 polypropylene Polymers 0.000 claims abstract description 8
- 229920001155 polypropylene Polymers 0.000 claims abstract description 8
- 239000000758 substrate Substances 0.000 claims description 49
- 239000003795 chemical substances by application Substances 0.000 claims description 43
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 36
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 24
- 239000007864 aqueous solution Substances 0.000 claims description 14
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 12
- 239000001103 potassium chloride Substances 0.000 claims description 6
- 235000011164 potassium chloride Nutrition 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 239000011159 matrix material Substances 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 3
- 238000011109 contamination Methods 0.000 abstract description 2
- 230000002829 reductive effect Effects 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 73
- 238000000034 method Methods 0.000 description 14
- 239000011259 mixed solution Substances 0.000 description 13
- 238000000926 separation method Methods 0.000 description 12
- 230000008569 process Effects 0.000 description 11
- 239000006228 supernatant Substances 0.000 description 8
- 229960005486 vaccine Drugs 0.000 description 7
- 241000251468 Actinopterygii Species 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 235000015277 pork Nutrition 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 230000002421 anti-septic effect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 206010002198 Anaphylactic reaction Diseases 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 206010061481 Renal injury Diseases 0.000 description 1
- 230000036783 anaphylactic response Effects 0.000 description 1
- 208000003455 anaphylaxis Diseases 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000021393 food security Nutrition 0.000 description 1
- 238000002649 immunization Methods 0.000 description 1
- 230000003053 immunization Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 208000037806 kidney injury Diseases 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 230000007472 neurodevelopment Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
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Abstract
The utility model relates to a pretreatment reagent kit for measuring thimerosal residues in animal derived food and belongs to the technical field of food safety. The pretreatment reagent kit for measuring thimerosal residues in the animal derived food is characterized by comprising a sample matrix extractant centrifuge tube, an acidity regulator centrifuge tube and a needle cylinder type filtration device. The sample matrix extractant centrifuge tube is a polypropylene centrifuge tube with a screw lid and a conical bottom, and the acidity regulator centrifuge tube is a centrifuge tube with a screw lid and a polypropylene conical bottom. The needle cylinder type filtration device is composed of a syringe needle tube and a needle type filter, wherein a filter membrane is positioned inside the needle type filter. The pretreatment reagent kit for measuring thimerosal residues in the animal derived food ensures that a form of thimerosal is not changed, thereby having the advantages of being high in extraction accuracy, high in extraction efficiency, small in used solvent quantity, simple and fast to operate, reductive in environmental contamination, beneficial for physical health of operating staffs and the like.
Description
Technical field
The utility model belongs to the food security technical field, particularly relates to the residual mensuration pretreatment reagent kit of thimerosal in a kind of animal derived food.
Background technology
At present, thimerosal (thimerosal) is a kind of mercurous organic compound, and mercurous in mass 49.6 % have the sterilizing effect, in the production of some vaccine, often are used as antiseptic.Since 1930, people use the thimerosal prevention vaccine by bacterium and other microbial contaminations.In whole immunization campaign process, except that possibly having slight cutaneous anaphylaxis, there is not the bad reaction that is attributable to thimerosal.Really, thimerosal has played great role to the security of vaccine for many years.Yet thimerosal has certain toxicity through injecting pathway to animal, and the shortage of xicity related effect and toxicity mechanism knowledge makes that the definite danger of thimerosal is difficult to confirm in the vaccine.But safety evaluatio can not be got rid of the baby and contact the possibility that the cumulative function of thimerosal in the vaccine causes the unusual and kidney injury of trickle neurodevelopment.No. the 235th, Ministry of Agriculture bulletin has stipulated that also thimerosal does vaccine antiseptic working concentration maximum and must not surpass 0.02 % in all food animals.Therefore, in order to guarantee the safety of animal derived food, the thimerosal residual quantity in the reply animal derived food detects.In the mensuration of prior art about thimerosal, all be to be directed against vaccine, also do not retrieve the detection method of thimerosal in the animal derived food matrix.Therefore, need set up a kind of method that detects thimerosal in the animal derived food matrix, also just need a kind of thimerosal rapidly and efficiently to extract the pretreatment technology device.
Summary of the invention
The utility model provides the residual mensuration pretreatment reagent kit of thimerosal in a kind of animal derived food for solving the problem that prior art exists.
The utility model purpose provides a kind of assurance thimerosal form and does not change; It is high to have the accuracy of extraction; Extraction efficiency is high, uses quantity of solvent few, and operating process is simple, quick; Reduce environmental pollution, helped the residual mensuration pretreatment reagent kit of thimerosal in the animal derived food of characteristics such as operating personnel are healthy.
The residual mensuration pretreatment reagent kit of thimerosal adopts following technical scheme in the utility model animal derived food:
The residual mensuration pretreatment reagent kit of thimerosal in a kind of animal derived food; Be characterized in: this kit comprises sample substrate extraction agent centrifuge tube, acidity regulator centrifuge tube and syringe-type filtration unit; Sample substrate extraction agent centrifuge tube is a tool plug screw top conical bottom polypropylene centrifuge tube; The acidity regulator centrifuge tube is a tool plug screw top polypropylene conical bottom centrifuge tube, and the needle tube type filtration unit is made up of syringe needle tube and needle-based filtrator, in the needle-based filtrator filter membrane is arranged.
The residual mensuration pretreatment reagent kit of thimerosal can also adopt following technical measures in the utility model animal derived food:
The residual mensuration pretreatment reagent kit of thimerosal in the described animal derived food; Be characterized in: sample substrate extraction agent centrifuge tube has 2, is respectively mixed aqueous solution centrifuge tube and hydrochloric acid, the thiocarbamide of potassium hydroxide, thiocarbamide, the mixed aqueous solution centrifuge tube of potassium chloride.
The residual mensuration pretreatment reagent kit of thimerosal in the described animal derived food is characterized in: sample substrate extraction agent centrifuge tube capacity is 30-70mL.
The residual mensuration pretreatment reagent kit of thimerosal in the described animal derived food, be characterized in: the acidity regulator centrifuge tube has 2, is respectively aqueous hydrochloric acid solution centrifuge tube and potassium hydroxide aqueous solution centrifuge tube.
The residual mensuration pretreatment reagent kit of thimerosal in the described animal derived food, be characterized in: acidity regulator centrifuge tube capacity is 30-70mL.
The residual mensuration pretreatment reagent kit of thimerosal in the described animal derived food is characterized in: syringe needle tube is the disposable syringe needle tubing of capacity 10-30mL.
The residual mensuration pretreatment reagent kit of thimerosal in the described animal derived food is characterized in: 0.3-0.8 μ m filter membrane is arranged in the needle-based filtrator.
Thimerosal selective extraction pre-treating method; Comprise: the animal derived food that contains thimerosal sample is provided, sample substrate extraction agent A, sample substrate extraction agent B, acidity regulator A, acidity regulator B and one-shot injector formula filtrator (containing 0.45 μ m filter membrane).
Said sample substrate extraction agent A, the animal derived food that contains thimerosal are pulverized sample to be mixed; Shake well obtains mixed solution, the centrifugal 5min of 10000r/min, and supernatant is transferred in the volumetric flask; Add sample substrate extraction agent B in the residue again; After fully mixing, centrifugal 5 min of 10000 r/min, supernatant is incorporated in the same volumetric flask.Acidity regulator A or B regulate the pH value, leave standstill 10 min behind the shake well, and thimerosal deposits sample plasma bottle in and supplies Instrument measuring in the said mixed solution after 0.45 μ m one-shot injector formula filtration unit filters.
Preferably, said sample substrate extraction agent A is the mixed aqueous solution of 5% potassium hydroxide and 0.5% thiocarbamide; Said sample substrate extraction agent B is the mixed aqueous solution of 20% hydrochloric acid, 1% thiocarbamide and 0.15% potassium chloride.
Preferably, the said acidity regulator A aqueous hydrochloric acid solution that is 0.1mol/L; Said acidity regulator B is the potassium hydroxide aqueous solution of 0.1mol/L.
Advantage that the utlity model has and good effect:
The residual mensuration pretreatment reagent kit of thimerosal in the animal derived food; Owing to adopted the utility model brand-new technology scheme; Compared with prior art, the sample pre-treatments kit extraction efficiency of thimerosal Selective Separation is high in the animal derived food sample that the utility model provides, and uses quantity of solvent few; Reduced environmental pollution, it is healthy to help operating personnel.
The sample pre-treatments kit advantage of thimerosal Selective Separation is in the animal derived food sample that the utility model provides: the sample substrate extraction agent A that 1) selects for use guarantees that to a certain extent the thimerosal form does not change, and has guaranteed the accuracy of extracting.2) select for use sample substrate extraction agent B extraction efficiency high.3) operating process is simple, quick, and this point is applicable to the quick pretreatment of thimerosal.
Description of drawings
Fig. 1 is the residual mensuration pretreatment reagent kit of a thimerosal structural representation in the utility model animal derived food;
The blank spectrogram that sample introduction after the thimerosal Selective Separation pretreatment reagent kit apparatus processes that Fig. 2 provides with the utility model for the pork sample substrate is analyzed;
The mark-on LC-AFS spectrogram that sample introduction after Fig. 3 thimerosal Selective Separation pretreatment reagent kit apparatus processes that to be the pork sample substrate provide with the utility model is analyzed;
The blank spectrogram that sample introduction after the thimerosal Selective Separation pretreatment reagent kit apparatus processes that Fig. 4 provides with the utility model for flesh of fish sample substrate is analyzed;
Fig. 5 is the mark-on LC-AFS spectrogram that the sample introduction after the thimerosal Selective Separation pretreatment reagent kit apparatus processes that provides with the utility model of flesh of fish sample substrate is analyzed.
Among the figure, 1-sample substrate extraction agent A, 2-sample substrate extraction agent B, 3-acidity regulator A, 4-acidity regulator B, the disposable needle tubing filtration unit 5 of 5-.
Embodiment
For further understanding technology contents, characteristics and the effect of the utility model, enumerate following instance now, and conjunction with figs. specifies as follows:
With reference to accompanying drawing 1 to Fig. 5.
The residual mensuration pretreatment reagent kit of thimerosal adopts following technical scheme in the utility model animal derived food:
The residual mensuration pretreatment reagent kit of thimerosal in a kind of animal derived food comprises 2 sample substrate extraction agent centrifuge tubes, 2 acidity regulator centrifuge tubes and a trocar barrel type filtering device.2 sample substrate extraction agent centrifuge tube A1, sample substrate extraction agent centrifuge tube B2 are tool plug screw top conical bottom polypropylene centrifuge tube, are respectively the mixed aqueous solution centrifuge tube of potassium hydroxide and thiocarbamide and the mixed aqueous solution centrifuge tube of hydrochloric acid, thiocarbamide and potassium chloride.2 acidity regulator centrifuge tube A3, acidity regulator centrifuge tube B4 are tool plug screw top polypropylene conical bottom centrifuge tube, are respectively aqueous hydrochloric acid solution and potassium hydroxide aqueous solution centrifuge tube.The needle tube type filtration unit is made up of shot device needle tubing 6 and needle-based filtrator 5, and 0.45 μ m filter membrane is arranged in the needle-based filtrator.
Details are as follows for the utility model composition and use thereof:
Thimerosal Selective Separation pretreatment reagent kit comprises sample substrate extraction agent A 1, sample substrate extraction agent B 2, acidity regulator A 3, acidity regulator B 4, disposable needle tubing filtration unit 5 in the animal derived food sample.Disposable needle tubing filtration unit syringe leading portion can closely cooperate with the filter membrane rear end.
Sample substrate extraction agent A guarantees that to a certain extent the thimerosal form does not change, and guaranteed the accuracy of extracting, but extraction efficiency is not high; Sample substrate extraction agent B extraction efficiency is high, but some thimerosal is converted into inorganic mercury in leaching process, causes morphological analysis inaccurate.Therefore extract with sample substrate extraction agent A earlier, remaining sample residue extracts with sample substrate extraction agent B again, can guarantee that the form of most of thimerosal is constant, also can reach higher extraction efficiency.Entering analytical instrument such as liquid chromatography-atomic fluorescence combined instrument were measured after disposable needle tube type filtration unit can filter sample solution.
The disposal route of thimerosal Selective Separation pretreatment reagent kit comprises in a kind of animal derived food sample:
The animal derived food that contains thimerosal sample is provided, sample substrate extraction agent A, sample substrate extraction agent B, acidity regulator A, acidity regulator B, disposable needle tubing filtration unit (containing 0.45 μ m filter membrane);
Said sample substrate extraction agent A, the animal derived food that contains thimerosal are pulverized sample to be mixed; Shake well obtains mixed solution, the centrifugal 5min of 10000r/min, and supernatant is transferred in the volumetric flask; Add sample substrate extraction agent B in the residue again; After fully mixing, centrifugal 5 min of 10000 r/min, supernatant is incorporated in the same volumetric flask.Acidity regulator A or B regulate the pH value, leave standstill 10 min behind the shake well, and said target mixed solution deposits sample plasma bottle in and supplies Instrument measuring after 0.45 μ m one-shot injector formula filtration unit filters.Target compound refers to thimerosal in the said mixed solution.
Said sample substrate extraction agent A can be 3%～7% potassium hydroxide and 0.3%～0.7% thiocarbamide mixed solution.
Said sample substrate extraction agent B can be 15%～25% hydrochloric acid, 0.7%～1.3% thiocarbamide and 0.1%～0.2% potassium chloride mixed solution.
Said sample acidity regulator A is the aqueous hydrochloric acid solution of 0.05mol/L～0.15mol/L.
Said sample acidity regulator B is the potassium hydroxide aqueous solution of 0.05mol/L～0.15mol/L.
Said one-shot injector formula filter for installation comprises 0.45 μ m filter membrane.
Specific operation process:
Pulverize adding sample substrate extraction agent A in the sample to the animal derived food that contains thimerosal, sample substrate extraction agent A is 3%～7% potassium hydroxide and 0.3%～0.7% thiocarbamide mixed solution, and shake well obtains mixed solution; The centrifugal 5min of 10000r/min; Supernatant is transferred in the volumetric flask; Add sample substrate extraction agent B in the residue again, sample substrate extraction agent B can be 15%～25% hydrochloric acid, 0.7%～1.3% thiocarbamide and 0.1%～0.2% potassium chloride mixed solution, after fully mixing; Centrifugal 5 min of 10000 r/min, supernatant is incorporated in the same volumetric flask.Regulate the pH value with acidity regulator A (aqueous hydrochloric acid solution of 0.05mol/L～0.15mol/L) or acidity regulator B (potassium hydroxide aqueous solution of 0.05mol/L～0.15mol/L); Leave standstill 10 min behind the shake well, thimerosal deposits sample plasma bottle in and supplies Instrument measuring in the said mixed solution after 0.45 μ m one-shot injector formula filtration unit filters.
The characteristics of this method are: sample substrate extraction agent A guarantees that to a certain extent the thimerosal form does not change; Guaranteed the accuracy of extracting; The extraction efficiency of sample substrate extraction agent B is high; Realized efficiently, thimerosal Selective Separation in the animal derived food sample fast, detect in order to follow-up liquid chromatography-atomic fluorescence combined instrument.
Concrete application example:
1, get thimerosal Selective Separation pretreatment reagent kit in the said animal derived food sample that the utility model provides, the inside is furnished with sample substrate extraction agent A, sample substrate extraction agent B, acidity regulator A, acidity regulator B and disposable needle tube type filtrator.
2, sample substrate extraction agent A, the animal derived food that contains thimerosal being pulverized sample mixes; Shake well obtains mixed solution, the centrifugal 5min of 10000r/min, and supernatant is transferred in the volumetric flask; Add sample substrate extraction agent B in the residue again; After fully mixing, centrifugal 5 min of 10000 r/min, supernatant is incorporated in the same volumetric flask.Acidity regulator A or B regulate the pH value; Leave standstill 10 min behind the shake well; Thimerosal deposits sample plasma bottle feed flow phase chromatogram-atomic fluorescence combined instrument (LC-AFS) mensuration in the said mixed solution after 0.45 μ m one-shot injector formula filtration unit filters, and extraction recovery reaches 70.0～86.2% as a result.
3, make an experiment with pork and flesh of fish article, the mark-on sample of preparation 0.1mg/kg, with 2 operations down, sample solution injects LC-AFS and measures.The result sees Fig. 2 to Fig. 5; The blank and the mark-on LC-AFS spectrogram of the sample introduction analysis after the thimerosal Selective Separation pretreatment reagent kit apparatus processes that blank and mark-on LC-AFS spectrogram that the sample introduction after the thimerosal Selective Separation pretreatment reagent kit apparatus processes that Fig. 2 and Fig. 3 provide with the utility model for the pork sample substrate is analyzed, Fig. 4 and Fig. 5 provide with the utility model for flesh of fish sample substrate.
Claims (7)
1. the residual mensuration pretreatment reagent kit of thimerosal in the animal derived food; It is characterized in that: this kit comprises sample substrate extraction agent centrifuge tube, acidity regulator centrifuge tube and syringe-type filtration unit; Sample substrate extraction agent centrifuge tube is a tool plug screw top conical bottom polypropylene centrifuge tube; The acidity regulator centrifuge tube is a tool plug screw top polypropylene conical bottom centrifuge tube, and the needle tube type filtration unit is made up of syringe needle tube and needle-based filtrator, in the needle-based filtrator filter membrane is arranged.
2. according to the residual mensuration pretreatment reagent kit of thimerosal in the described animal derived food of claim 1; It is characterized in that: sample substrate extraction agent centrifuge tube has 2, is respectively mixed aqueous solution centrifuge tube and hydrochloric acid, the thiocarbamide of potassium hydroxide, thiocarbamide, the mixed aqueous solution centrifuge tube of potassium chloride.
3. according to the residual mensuration pretreatment reagent kit of thimerosal in claim 1 or the 2 described animal derived foods, it is characterized in that: sample substrate extraction agent centrifuge tube capacity is 30-70mL.
4. according to the residual mensuration pretreatment reagent kit of thimerosal in the described animal derived food of claim 1, it is characterized in that: the acidity regulator centrifuge tube has 2, is respectively aqueous hydrochloric acid solution centrifuge tube and potassium hydroxide aqueous solution centrifuge tube.
5. according to the residual mensuration pretreatment reagent kit of thimerosal in claim 1 or the 4 described animal derived foods, it is characterized in that: acidity regulator centrifuge tube capacity is 30-70mL.
6. according to the residual mensuration pretreatment reagent kit of thimerosal in the described animal derived food of claim 1, it is characterized in that: syringe needle tube is the disposable syringe needle tubing of capacity 10-30mL.
7. according to the residual mensuration pretreatment reagent kit of thimerosal in the described animal derived food of claim 1, it is characterized in that: 0.3-0.8 μ m filter membrane is arranged in the needle-based filtrator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011204468258U CN202471663U (en) | 2011-11-14 | 2011-11-14 | Pretreatment reagent kit for measuring thimerosal residues in animal derived food |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011204468258U CN202471663U (en) | 2011-11-14 | 2011-11-14 | Pretreatment reagent kit for measuring thimerosal residues in animal derived food |
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| Publication Number | Publication Date |
|---|---|
| CN202471663U true CN202471663U (en) | 2012-10-03 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011204468258U Expired - Fee Related CN202471663U (en) | 2011-11-14 | 2011-11-14 | Pretreatment reagent kit for measuring thimerosal residues in animal derived food |
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| Country | Link |
|---|---|
| CN (1) | CN202471663U (en) |
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2011
- 2011-11-14 CN CN2011204468258U patent/CN202471663U/en not_active Expired - Fee Related
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20121003 Termination date: 20141114 |
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| EXPY | Termination of patent right or utility model |