CN111505272A - Excrement diluent and application thereof - Google Patents

Excrement diluent and application thereof Download PDF

Info

Publication number
CN111505272A
CN111505272A CN202010311488.5A CN202010311488A CN111505272A CN 111505272 A CN111505272 A CN 111505272A CN 202010311488 A CN202010311488 A CN 202010311488A CN 111505272 A CN111505272 A CN 111505272A
Authority
CN
China
Prior art keywords
diluent
percent
mass
sample
stool
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
Application number
CN202010311488.5A
Other languages
Chinese (zh)
Inventor
田颖
张少丹
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shijiazhuang Huanzhong Biotechnology Co ltd
Original Assignee
Shijiazhuang Huanzhong Biotechnology Co ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shijiazhuang Huanzhong Biotechnology Co ltd filed Critical Shijiazhuang Huanzhong Biotechnology Co ltd
Priority to CN202010311488.5A priority Critical patent/CN111505272A/en
Publication of CN111505272A publication Critical patent/CN111505272A/en
Pending legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/48Biological material, e.g. blood, urine; Haemocytometers
    • G01N33/50Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
    • G01N33/53Immunoassay; Biospecific binding assay; Materials therefor
    • G01N33/531Production of immunochemical test materials
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/48Biological material, e.g. blood, urine; Haemocytometers
    • G01N33/50Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
    • G01N33/53Immunoassay; Biospecific binding assay; Materials therefor
    • G01N33/558Immunoassay; Biospecific binding assay; Materials therefor using diffusion or migration of antigen or antibody

Abstract

The invention belongs to the technical field of sample diluent preparation, and relates to a stool diluent and application thereof. The excrement diluent comprises the following components in percentage by mass: 5 to 10 percent of buffer solution, 0.02 to 0.06 percent of surfactant, 0.005 to 0.02 percent of bacteriostatic agent, 0.02 to 0.06 percent of bovine serum albumin and the balance of distilled water. The excrement diluent provided by the invention is low in cost, can effectively improve the stability of a diluent system, prevents bacterial pollution, does not influence the components of a sample, has no interference on a detection result, can be better used for immunochromatography rapid detection and analysis, avoids the occurrence of nonspecific adsorption reaction of the sample, and ensures the repeatability and accuracy of the detection result.

Description

Excrement diluent and application thereof
Technical Field
The invention relates to the technical field of sample diluent preparation, in particular to a stool diluent and application thereof.
Background
Human feces mainly comprise undigested food, food which is not absorbed after digestion, secretion of a digestive system, digestive tract mucosa castoff, microorganisms, parasites and the like, and the human feces are detected to obtain information of digestive system functions, pathological changes, microorganism infection, parasite infection and the like of a detected person. When testing and assaying the feces, the feces usually needs to be diluted by a feces diluent.
Most of the existing excrement diluent is tap water, deionized water and normal saline, the tap water and the deionized water cannot protect the form of visible components in excrement, and the change of the form of the components with diagnostic significance can influence the judgment of the routine diagnostic result of the excrement; in addition, tap water and deionized water are used as diluents, and the positive detection rate is low when the diluents are used for an immunochromatography fecal occult blood test. The normal saline is generally used for manual detection, and the normal saline is not subjected to bacteriostatic treatment, so that microorganisms are bred in the pipeline if the normal saline is used in a matched excrement analysis workstation, and the pipeline is possibly blocked due to crystallization after long-term use, so that the normal saline is not suitable for instruments. Therefore, the conventional use of water or physiological saline as a stool diluent is disadvantageous to the stability of the reaction system and is easily contaminated, thereby affecting the judgment of the result. Moreover, if only the buffer solution and the bacteriostatic agent are added into the diluent, the specific adsorption reaction of the sample cannot be inhibited, and the judgment of the detection result is also affected. Therefore, providing a stool diluent that does not affect the form of sample components and can avoid non-specific adsorption reactions of the sample is important for obtaining information such as digestive system function, pathological changes, microbial and parasitic infections of a detector in stool detection and assay.
Disclosure of Invention
In view of the above, the invention provides the stool diluent and the application thereof, and the stool diluent can effectively improve the stability of a diluent system, does not affect the components of a sample, avoids the occurrence of nonspecific adsorption reaction of the sample, and ensures the repeatability and the accuracy of a detection result.
In order to solve the technical problems, the invention provides the following technical scheme:
the invention provides a feces diluent which comprises the following components in percentage by mass: 5 to 10 percent of buffer substance, 0.02 to 0.06 percent of surfactant, 0.005 to 0.02 percent of bacteriostatic agent, 0.02 to 0.06 percent of bovine serum albumin and the balance of distilled water.
Preferably, the buffer substance is a disodium hydrogen phosphate-potassium dihydrogen phosphate mixture or a tris-sodium chloride mixture.
More preferably, when the buffer substance is a mixture of disodium hydrogen phosphate and potassium dihydrogen phosphate, the content of disodium hydrogen phosphate in the feces diluent is 5 to 7% by mass, and the content of potassium dihydrogen phosphate in the feces diluent is 0.5 to 1.5% by mass.
More preferably, when the buffer substance is a tris-sodium chloride mixture, the tris is 8 to 10% by mass in the feces diluent and the sodium chloride is 0.5 to 0.8% by mass in the feces diluent.
Preferably, the surfactant is Tween-80.
More preferably, the mass percentage of the Tween-80 in the feces diluent is 0.05%.
Preferably, the bacteriostatic agent is sodium benzoate.
More preferably, the sodium benzoate accounts for 0.01 percent of the mass of the excrement diluent.
Preferably, the bovine blood albumin is 0.05% by mass of the feces diluent.
The invention also provides application of the excrement diluent in excrement detection assay.
Compared with the prior art, the invention has the following beneficial effects:
the excrement diluent comprises a buffer substance, a surfactant, a bacteriostatic agent and bovine serum albumin, wherein the surfactant can provide a good hydrophilic environment for sample reaction, so that a sample can be fully dissolved, the buffer solution can improve the ionic environment of the sample, and the buffer solution and the bovine serum albumin added at the same time can prevent the sample from generating nonspecific adsorption reaction and have a certain pH buffering effect on the sample. The excrement diluent provided by the invention is low in cost, can effectively improve the stability of a diluent system, prevents bacterial pollution, does not influence the components of a sample, has no interference on a detection result, can be better used for immunochromatography rapid detection and analysis, avoids the occurrence of nonspecific adsorption reaction of the sample, and ensures the repeatability and accuracy of the detection result.
Detailed Description
The invention provides a feces diluent which comprises the following components in percentage by mass: 5 to 10 percent of buffer substance, 0.02 to 0.06 percent of surfactant, 0.005 to 0.02 percent of bacteriostatic agent, 0.02 to 0.06 percent of bovine serum albumin and the balance of distilled water.
In the present invention, the buffer substance is preferably a disodium hydrogen phosphate-potassium dihydrogen phosphate mixture or a tris-sodium chloride mixture. The content of the buffer substance in percentage by mass is preferably 5% -10%, and more preferably 6% -8%. In the invention, the buffer substance mainly functions to improve the ionic environment of the sample and provide a stable pH environment, thereby providing a stable reaction system for the sample.
In the present invention, when the buffer substance is a disodium hydrogen phosphate-potassium dihydrogen phosphate mixture, the content of disodium hydrogen phosphate in the feces diluent is preferably 5% to 7% by mass, and more preferably 6% by mass; the content of monopotassium phosphate in the feces diluent is preferably 0.5-1.5% by mass, and more preferably 1% by mass. When the buffer substance is a tris-sodium chloride mixture, the mass percentage content of tris in the feces diluent is preferably 8% -10%, more preferably 9%; the mass percentage content of the sodium chloride in the feces diluent is preferably 0.5-0.8%, and more preferably 0.6%. The sources of the disodium hydrogen phosphate, the potassium dihydrogen phosphate, the tris (hydroxymethyl) aminomethane and the sodium chloride are not particularly limited in the present invention, and any commercially available product that is conventional in the art may be used.
In the invention, the surfactant is preferably Tween-80. The mass percentage content of the surfactant in the feces diluent is preferably 0.02-0.06%, and more preferably 0.05%. In the invention, the Tween-80 has excellent water solubility and mainly plays a role in providing a good hydrophilic environment for sample reaction so as to enable the sample to be fully dissolved. The source of the Tween-80 is not particularly limited in the invention, and the Tween-80 can be prepared from conventional commercial products in the field.
In the invention, the bacteriostatic agent is preferably sodium benzoate. The mass percentage content of the sodium benzoate in the excrement diluent is preferably 0.005% -0.02%, and more preferably 0.01%. In the invention, the bacteriostatic agent has the functions of preventing a reaction system from being polluted by bacteria and prolonging the preservation time of the diluent. The source of the sodium benzoate is not particularly limited in the invention, and the conventional commercial products in the field can be adopted.
In the invention, the bovine blood albumin is preferably newborn bovine blood serum. The bovine blood albumin is preferably 0.02 to 0.06 percent by mass, and more preferably 0.05 percent by mass in the feces diluent. In the invention, the bovine blood albumin can not only prevent the sample from generating nonspecific adsorption reaction, but also play a certain role in pH buffering for the sample. The source of the present invention is not particularly limited, and any commercially available product conventionally used in the art may be used.
In the present invention, the distilled water is used as a solvent. The addition amount of the distilled water is not particularly limited, and the amount can be specifically adjusted according to the total amount of the excrement diluent required by preparation and the mass percentage of each component.
The invention also provides application of the excrement diluent in excrement detection assay. The excrement diluent disclosed by the invention is used for diluting excrement and detecting and testing the diluted excrement to obtain excrement related information.
In order to further illustrate the present invention, the following embodiments are described in detail, but they should not be construed as limiting the scope of the present invention.
In this example, other materials or instruments are commercially available, and the source thereof is not limited in the present invention.
Example 1
The components are as follows by mass percent: 6 percent of disodium hydrogen phosphate, 1 percent of monopotassium phosphate, 1 percent of Tween-800.05, 0.01 percent of sodium benzoate and 0.05 percent of bovine blood albumin, and dissolving the mixture in distilled water to prepare the excrement diluent.
Example 2
The components are as follows by mass percent: 7 percent of disodium hydrogen phosphate, 0.5 percent of monopotassium phosphate, 0.01 percent of Tween-800.05 percent of sodium benzoate and 0.05 percent of bovine blood albumin, and dissolving the components in distilled water to prepare the excrement diluent.
Example 3
The components are as follows by mass percent: 7 percent of disodium hydrogen phosphate, 1.5 percent of monopotassium phosphate, 1.78 percent of Tween-800.05 percent, 0.01 percent of sodium benzoate and 0.05 percent of bovine blood albumin, and dissolving the mixture in distilled water to prepare the excrement diluent.
Example 4
The components are as follows by mass percent: 8% of trihydroxymethyl aminomethane, 0.5% of sodium chloride, 0.78% of Tween-800.05%, 0.01% of sodium benzoate and 0.05% of bovine blood albumin, and dissolving in distilled water to prepare the feces diluent.
Example 5
The components are as follows by mass percent: 9 percent of trihydroxymethyl aminomethane, 0.6 percent of sodium chloride, 0.01 percent of Tween-800.05 percent of sodium benzoate and 0.05 percent of bovine blood albumin are dissolved in distilled water to prepare the excrement diluent.
Example 6
The components are as follows by mass percent: 10 percent of trihydroxymethyl aminomethane, 0.8 percent of sodium chloride, 0.01 percent of Tween-800.05 percent of sodium benzoate and 0.05 percent of bovine blood albumin are dissolved in distilled water to prepare the excrement diluent.
Example 7
1. Erythrocyte deformation and rupture rate measurement
The fecal diluent 10m L prepared in the above examples 1-6 was put into a test tube, 50 μ L of red blood cell sample was added to the test tube, mixed, 2-3 drops of the sample was dropped into a cell counting plate, mixed, the total amount and morphological abnormality number of red blood cells in the counting frame of the cell counting plate were counted using a biological microscope, and the deformation rate and rupture rate of red blood cells were calculated according to the following formulas, and the results are shown in table 1.
Erythrocyte morphosis rate (%) -abnormal morphology erythrocyte number ÷ total erythrocyte number × 100%
TABLE 1 Effect of stool dilution on erythrocyte deformation and rupture Rate
Numbering Percent deformation (%) Percentage of rupture (%)
Example 1 1 0
Example 2 2 1
Example 3 2 0
Example 4 1 1
Example 5 1 0
Example 6 1 1
The above results show that: the fecal dilutions of examples 1-6 had low erythrocyte deformation rates, and were able to maintain erythrocyte morphology well, without affecting the composition of the sample itself, and without interfering with the assay results.
2. Stability test
The stool dilutions 10m L prepared in the above examples 1-6 were used as experimental group and 10m L0.9.9% physiological saline as control group, and the experimental group and the control group were placed in the same indoor environment for three months, and the conditions of the experimental group and the control group were observed every month, and the experimental results were recorded as shown in table 2:
TABLE 2 contamination of the fecal dilutions over time
Numbering One month Two months old Three months old
Example 1 Clear and transparent without foreign matter Clear and transparent without foreign matter Clear and transparent without foreign matter
Example 2 Clear and transparent without foreign matter Clear and transparent without foreign matter Clear and transparent without foreign matter
Example 3 Clear and transparent without foreign matter Clear and transparent without foreign matter Clear and transparent without foreign matter
Example 4 Clear and transparent without foreign matter Clear and transparent without foreign matter Clarifying and penetratingHas no foreign matter
Example 5 Clear and transparent without foreign matter Clear and transparent without foreign matter Clear and transparent without foreign matter
Example 6 Clear and transparent without foreign matter Clear and transparent without foreign matter Clear and transparent without foreign matter
Control group Clear and transparent without foreign matter Slightly flocculent Has more floccules
From the above results, it can be seen that: the fecal diluent prepared in the examples 1-6 of the invention has no obvious change, while the normal saline control group gradually generates floccules. The excrement diluent can prevent bacterial pollution and has good stability.
3. Repeatability and accuracy testing
The stool diluent is tested by utilizing a conventional commercially available immunochromatographic test strip in the field, and the accuracy of the diluent is verified by using an automatic stool analyzer as a reference.
Taking out the immunochromatographic assay plate, and placing the immunochromatographic assay plate on a drying platform.
10 portions of each of the positive fecal sample and the negative fecal sample are diluted to be completely dissolved by the fecal diluent prepared in the above example 1, 3 to 4 drops of the sample floating on the upper layer are absorbed and added into the sample adding hole of the immunochromatographic detection plate, and the result is read after 10 minutes. At the same time, a stool analyzer was used for the control test. The following table 3 was obtained:
TABLE 3 dilution test results of different samples with stool diluent
Figure BDA0002457773860000061
Figure BDA0002457773860000071
As can be seen from the above table, the test results of the sample diluent combined with the test strip are consistent with the theoretical values, and the repeated results are consistent, which shows that the stool diluent of the invention has no interference to the test results and has repeatability. Meanwhile, the detection result of the excrement diluent combined with the test strip is consistent with that of an excrement analyzer, and the excrement diluent has good accuracy.
The embodiment shows that the excrement diluent provided by the invention is low in cost, can effectively improve the stability of a diluent system, prevents bacterial pollution, does not influence the components of a sample, has no interference on a detection result, can be better used for immunochromatography rapid detection and analysis, avoids the occurrence of nonspecific adsorption reaction of the sample, and ensures the repeatability and accuracy of the detection result.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.

Claims (10)

1. The excrement diluent is characterized by comprising the following components in percentage by mass: 5 to 10 percent of buffer substance, 0.02 to 0.06 percent of surfactant, 0.005 to 0.02 percent of bacteriostatic agent, 0.02 to 0.06 percent of bovine serum albumin and the balance of distilled water.
2. Faecal dilution according to claim 1, characterised in that the buffer substance is a mixture of disodium hydrogen phosphate and potassium dihydrogen phosphate or a mixture of tris-sodium chloride.
3. The stool dilution according to claim 2, wherein when the buffer substance is a disodium hydrogen phosphate-potassium dihydrogen phosphate mixture, the disodium hydrogen phosphate is present in the stool dilution in an amount of 5% to 7% by mass, and the potassium dihydrogen phosphate is present in the stool dilution in an amount of 0.5% to 1.5% by mass.
4. The diluted feces liquid according to claim 2, wherein when the buffer substance is a tris-sodium chloride mixture, tris is present in an amount of 8 to 10% by mass in the diluted feces liquid, and sodium chloride is present in an amount of 0.5 to 0.8% by mass in the diluted feces liquid.
5. The fecal diluent of claim 1 wherein the surfactant is Tween-80.
6. The fecal diluent of claim 5, characterized in that the mass percentage content of Tween-80 in the fecal diluent is 0.05%.
7. The fecal diluent of claim 1 wherein the bacteriostatic agent is sodium benzoate.
8. The stool dilution according to claim 7, wherein the sodium benzoate is present in the stool dilution in an amount of 0.01% by weight.
9. The stool dilution according to claim 1, wherein the bovine blood albumin is present in the stool dilution in an amount of 0.05% by weight.
10. Use of a stool dilution according to any one of claims 1-9 in a stool detection assay.
CN202010311488.5A 2020-04-20 2020-04-20 Excrement diluent and application thereof Pending CN111505272A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010311488.5A CN111505272A (en) 2020-04-20 2020-04-20 Excrement diluent and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010311488.5A CN111505272A (en) 2020-04-20 2020-04-20 Excrement diluent and application thereof

Publications (1)

Publication Number Publication Date
CN111505272A true CN111505272A (en) 2020-08-07

Family

ID=71876219

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010311488.5A Pending CN111505272A (en) 2020-04-20 2020-04-20 Excrement diluent and application thereof

Country Status (1)

Country Link
CN (1) CN111505272A (en)

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5094956A (en) * 1987-02-04 1992-03-10 International Immunoassay Laboratories, Inc. Fecal sample immunoassay composition and method
US20010024801A1 (en) * 1999-04-15 2001-09-27 Nair Padmanabhan P. Noninvasive detection of colorectal cancer and other gastrointestinal pathology
JP2007322310A (en) * 2006-06-02 2007-12-13 Nippon Kayaku Co Ltd Method for detecting or measuring substance to be analyzed in specimen
CN106769289A (en) * 2016-12-02 2017-05-31 刘鹏飞 A kind of collocation method of fecal specimens storage liquid and application
CN108982199A (en) * 2018-08-13 2018-12-11 湖南品信生物工程有限公司 A kind of excrement dilution
CN109557088A (en) * 2019-01-11 2019-04-02 四川沃文特生物技术有限公司 A kind of reagent card for detecting excrement lactose content and the excrement lactose detection method based on this
CN109679769A (en) * 2018-12-14 2019-04-26 湖南品信生物工程有限公司 A kind of excrement cleaning solution for excrement detector
CN110320364A (en) * 2018-03-30 2019-10-11 洛阳普莱柯万泰生物技术有限公司 A kind of double antibodies sandwich gold-immunochromatographyreagent reagent for assay box, and the preparation method and application thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5094956A (en) * 1987-02-04 1992-03-10 International Immunoassay Laboratories, Inc. Fecal sample immunoassay composition and method
US20010024801A1 (en) * 1999-04-15 2001-09-27 Nair Padmanabhan P. Noninvasive detection of colorectal cancer and other gastrointestinal pathology
JP2007322310A (en) * 2006-06-02 2007-12-13 Nippon Kayaku Co Ltd Method for detecting or measuring substance to be analyzed in specimen
CN106769289A (en) * 2016-12-02 2017-05-31 刘鹏飞 A kind of collocation method of fecal specimens storage liquid and application
CN110320364A (en) * 2018-03-30 2019-10-11 洛阳普莱柯万泰生物技术有限公司 A kind of double antibodies sandwich gold-immunochromatographyreagent reagent for assay box, and the preparation method and application thereof
CN108982199A (en) * 2018-08-13 2018-12-11 湖南品信生物工程有限公司 A kind of excrement dilution
CN109679769A (en) * 2018-12-14 2019-04-26 湖南品信生物工程有限公司 A kind of excrement cleaning solution for excrement detector
CN109557088A (en) * 2019-01-11 2019-04-02 四川沃文特生物技术有限公司 A kind of reagent card for detecting excrement lactose content and the excrement lactose detection method based on this

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
吴丹等: "一种快速检测粪便中血红蛋白的胶体金方法", 《江西中医药大学学报》 *

Similar Documents

Publication Publication Date Title
Sutton Evaluation of hematuria in adults
JP2763635B2 (en) Detection of diamines in biological fluids
Graham et al. ACP Best Practice No 167: the laboratory diagnosis of urinary tract infection
Flanagan et al. Evaluation of four screening tests for bacteriuria in elderly people
Yermak et al. Performance of synovial fluid D-lactate for the diagnosis of periprosthetic joint infection: A prospective observational study
Leung et al. False-negative biopsy urease test in bleeding ulcers caused by the buffering effects of blood
Terčelj et al. Fungal exposure in homes of patients with sarcoidosis-an environmental exposure study
CN107727869A (en) Kit of antinuclear antibodies and preparation method thereof in a kind of measure serum
CN110129406A (en) A kind of pseudomonas aeruginosa chromogenic culture medium and the method quickly detected using it
Zagra et al. Can leucocyte esterase replace frozen sections in the intraoperative diagnosis of prosthetic hip infection?
Sharief et al. Use of rapid dipstick tests to exclude urinary tract infectionin children
Gasol et al. Cytometric evidence reconciling the toxicity and usefulness of CTC as a marker of bacterial activity
Wu et al. Association between fluoride exposure and kidney function in adults: A cross-sectional study based on endemic fluorosis area in China
Broeren et al. Urine flow cytometry is an adequate screening tool for urinary tract infections in children
CN111505272A (en) Excrement diluent and application thereof
Halliday et al. Giardia-bile salt interactions in vitro and in vivo
CN108982199A (en) A kind of excrement dilution
Wacker et al. The Holy Cross hepatitis outbreak: Clinical and chemical abnormalities
Sawyer et al. Evaluation of a leukocyte dip-stick test used for screening urine cultures
CN101706508A (en) Preparation method of ABO subtype detection kit
Simmons An automated method for serum bilirubin determination
Thysell Evaluation of chemical and microscopical methods for mass detection of bacteriuria
EP0178501B1 (en) Method for detection of peritoneal inflammation or infection
Uwamino et al. Efficient automated semi-quantitative urine culture analysis via BD Urine Culture App
Al-Daghistani et al. Diagnostic value of various urine tests in the Jordanian population with urinary tract infection

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20200807

RJ01 Rejection of invention patent application after publication