CN110470664A - Quickly determine preparation method of the test to picture ID of residues of organophosphate pesticides content - Google Patents
Quickly determine preparation method of the test to picture ID of residues of organophosphate pesticides content Download PDFInfo
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- CN110470664A CN110470664A CN201910781490.6A CN201910781490A CN110470664A CN 110470664 A CN110470664 A CN 110470664A CN 201910781490 A CN201910781490 A CN 201910781490A CN 110470664 A CN110470664 A CN 110470664A
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- 238000012360 testing method Methods 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000575 pesticide Substances 0.000 title claims abstract description 14
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000011574 phosphorus Substances 0.000 claims abstract description 24
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 23
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000003085 diluting agent Substances 0.000 claims abstract description 5
- 239000008055 phosphate buffer solution Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 abstract description 14
- 230000000903 blocking effect Effects 0.000 abstract 1
- 238000001514 detection method Methods 0.000 description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 238000010790 dilution Methods 0.000 description 10
- 239000012895 dilution Substances 0.000 description 10
- 125000005461 organic phosphorous group Chemical group 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 239000012153 distilled water Substances 0.000 description 8
- LCCNCVORNKJIRZ-UHFFFAOYSA-N parathion Chemical compound CCOP(=S)(OCC)OC1=CC=C([N+]([O-])=O)C=C1 LCCNCVORNKJIRZ-UHFFFAOYSA-N 0.000 description 8
- 239000007788 liquid Substances 0.000 description 6
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 5
- 235000019796 monopotassium phosphate Nutrition 0.000 description 5
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- RLBIQVVOMOPOHC-UHFFFAOYSA-N parathion-methyl Chemical group COP(=S)(OC)OC1=CC=C([N+]([O-])=O)C=C1 RLBIQVVOMOPOHC-UHFFFAOYSA-N 0.000 description 4
- 239000000447 pesticide residue Substances 0.000 description 4
- 102000004190 Enzymes Human genes 0.000 description 3
- 108090000790 Enzymes Proteins 0.000 description 3
- 239000007853 buffer solution Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229940088598 enzyme Drugs 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 230000005764 inhibitory process Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000003987 organophosphate pesticide Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 102000012440 Acetylcholinesterase Human genes 0.000 description 2
- 108010022752 Acetylcholinesterase Proteins 0.000 description 2
- 229960004373 acetylcholine Drugs 0.000 description 2
- 229940022698 acetylcholinesterase Drugs 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 238000003018 immunoassay Methods 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- -1 phosphonothiolic acid esters organic compound Chemical class 0.000 description 2
- 206010008428 Chemical poisoning Diseases 0.000 description 1
- 208000012902 Nervous system disease Diseases 0.000 description 1
- VYRDHRYMAZWQJH-UHFFFAOYSA-N [P].P Chemical compound [P].P VYRDHRYMAZWQJH-UHFFFAOYSA-N 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- OIPILFWXSMYKGL-UHFFFAOYSA-N acetylcholine Chemical compound CC(=O)OCC[N+](C)(C)C OIPILFWXSMYKGL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000005875 antibody response Effects 0.000 description 1
- 239000000427 antigen Substances 0.000 description 1
- 102000036639 antigens Human genes 0.000 description 1
- 108091007433 antigens Proteins 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 208000015114 central nervous system disease Diseases 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 239000002329 esterase inhibitor Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 210000000232 gallbladder Anatomy 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 230000007830 nerve conduction Effects 0.000 description 1
- 231100000189 neurotoxic Toxicity 0.000 description 1
- 230000002887 neurotoxic effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention discloses a kind of tests of quick determining residues of organophosphate pesticides content to the preparation method of picture ID, and this method uses the phosphate buffer solution of pH 7.2-8.0 as diluent, will be diluted to concentration 0.2 × 10 with the dissolved organic phosphorus standard items of acetonitrile‑4~0.2 × 10‑2Then organic phosphorus solution of various concentration is added drop-wise in the residual test card of agriculture by organic phosphorus solution of the various concentration within the scope of mg/mL, while a diluent is added dropwise as blank control, and after the residual test card colour developing of agriculture, concentration is 0.2 × 10‑4~0.2 × 10‑2Multiple residual test cards of colour developing agriculture within the scope of mg/mL are to test to picture ID；The present invention can quickly determine the approximate range of residues of organophosphate pesticides content in sample to be tested, and present invention control blocking Preparation Method is simple, is suitable for outdoor and laboratory quick comparison, has a good application prospect.
Description
Technical field
The invention belongs to organic phosphorus in residues of organophosphate pesticides detection technique field more particularly to a kind of quick determining test substance
Preparation method of the test of the residual content approximate range of agriculture to picture ID.
Background technique
Along with economic development, requirement of the people to levels of substance is higher and higher, the Pesticide Residue in food also by
Gradually it is concerned.Organophosphorus pesticide typically refers to phosphorus (phosphine) acid esters or phosphonothiolic acid esters organic compound, comes out so far certainly
Have decades because efficiently, quickly, wide spectrum the features such as, occupy critically important position in pesticide always, usage amount accounts for about entirely
The 70% of portion's pesticide, but also environment is caused while its promotion agricultural development and centainly pollutes and seriously affected food safety,
Organophosphorus pesticide is a kind of neurotoxic substance, largely organic phosphorus that internal acetylcholinesterase can be made to inactivate, and human body is made to be poisoned
Symptom, especially central nervous system disorder, so that threat to life.
The common detection method of organophosphorus pesticide specifically includes that spectroscopic methodology, chromatography and mass spectrography etc. pass at present
The system rapid detection methods such as detection method and enzyme inhibition, immunoassay.The tradition such as spectroscopic methodology, chromatography and mass spectrography have
Machine phosphorus detection method, detection accuracy is high, can enforce the law for pesticide residue and provide foundation, but detection time is long, at high cost and not applicable
It is detected in when participating in the cintest.Fast Determination of Pesticide Residue method is the method for a kind of fast detecting pesticide residue, and immunoassays are to utilize antigen
The method that antibody response detects micro substance in sample, although the method is quick, high sensitivity, easy to operate, Antibody preparation hardly possible
Degree is big and is adapted only to single Detecting Pesticide.So needing to press down by with enzyme in face of the screening of a large amount of samples and on-site test
Preparation method is the residual detection card of agriculture of principle, and this method provides a kind of easy, sensitive, quick, economical for detection of organic phosphorus pesticide
Detection means, and enzyme inhibition is supported without Large expensive instrument, is suitable for the screening of a large amount of samples and on-site test.
But currently, the residual detection of normal agriculture, which blocks, can only detect whether have agriculture residual in substance, and the residual content of agriculture must not
And know, and in the detection process the dripping quantity of prepare liquid without significantly regulation so that be easy to appear the uneven situation of colour developing,
Detection effect is influenced, therefore, this problems demand improves, and the present invention compensates for this deficiency, it is pushed preferably to develop.
Summary of the invention
For the screening of a large amount of samples and on-site test demand, the present invention provides a kind of quick determining residues of organophosphate pesticides and substantially contains
Measure preparation method of the test to picture ID of range；The present invention uses the phosphate buffer solution of pH 7.2-8.0 as diluent, will
Concentration is diluted to 0.2 × 10 with the dissolved organic phosphorus standard items of acetonitrile-4~0.2 × 10-2Difference within the scope of mg/mL is dense
Organic phosphorus solution of various concentration, is then added drop-wise in the residual test card of agriculture by organic phosphorus solution of degree, while a dilution is added dropwise
Agent is as blank control, and after the residual test card colour developing of agriculture, concentration is 0.2 × 10-4~0.2 × 10-2It is multiple within the scope of mg/mL
The residual test card of agriculture that develops the color is to test to picture ID.
The method of the present invention solves the problems, such as that the residual detection card of conventional agriculture can not determine the residual substantially content of agriculture；Side through the invention
Method is simultaneously blocked using the residual detection of existing agriculture, can be produced for different one group of organic phosphorus color measurement to picture ID, from control
The color of card may determine that the concentration range of sample to be tested, the method for the present invention have universality；Present invention process is simple, is easy to
Operation；It is suitble to industrialized production after being made into finished product；Can be qualitative, and can quantify.
Wherein organic phosphorus standard items are first made into the solution of 0.1-0.2mg/mL with acetonitrile.
The phosphate buffer solution is the solution for the pH 7.2-8.0 that routinely scheme is prepared.
The residual test card of agriculture used in preparation method of the present invention is conventional commercial for different organic phosphorus colour developing cards.
It is described the organic phosphorus solution of various concentration to be added dropwise and the residual test card of agriculture of blank control liquid stands 10- at room temperature
After 15min, then with finger 3min is pinched, so far colour developing is completed.
Basic principle of the invention:
Colour developing principle of the invention is based on acetylcholine ester enzymatic nerve conduction metabolite (acetyl gallbladder in the residual detection card of agriculture
Alkali) hydrolysis, hydrolysate reacted with color developing agent generation color change, and it is organic phosphorus can with the activity of acetylcholine esterase inhibition,
And the organic phosphorus inhibiting rate to acetylcholinesterase and organic phosphorus amount are proportional, and the color depth of card is finally detected with inhibition
The increase of rate and lighter, the color burn with the reduction of inhibiting rate block so as to establish organic phosphorous content amount and detection
Corresponding relationship between display color weight, and one group of color is obtained by being deep to the control of shallow (organic phosphorous content is from low to high)
Card solves the problems, such as that the residual detection card of agriculture can not determine sample to be tested substantially content (quantitative).
Compared with prior art, the beneficial effects of the present invention are:
1, the shortcomings that existing residues of organophosphate pesticides detection card not can determine that organic phosphorous content range in determinand in the market is compensated for,
Quantitative detection can prevent the generation of pesticide poisoning event；
2, preparation process of the present invention is simply controllable, low to material requirements and the requirement of operator's specialized capability, and production cost is low, fits
For large-tonnage product come personally quantitative detection compare；
3, the present invention can be qualitative to residues of organophosphate pesticides, and can quantify；
4, product of the present invention detection effect is good, and preparation method is simple, is suitble to industrialized production, pushes the development of the residual detection industry of agriculture.
Specific embodiment
The invention will be further described for son combined with specific embodiments below, but the present embodiment is not limited in detail below
Embodiment.
Embodiment 1: phonamiphos tests the preparation method to picture ID, and concrete operations are as follows:
(1) phonamiphos standard items powder is taken, acetonitrile dissolution is added to be made into the solution of 0.104mg/mL；
(2) preparation of dilution: taking potassium dihydrogen phosphate 13.61g, adds distilled water to make it dissolve and is settled to 500mL with distilled water
The potassium dihydrogen phosphate for obtaining 0.2mol/L, takes 4g sodium hydroxide, adds distilled water to make it dissolve and be settled to 500mL with distilled water
The sodium hydroxide solution for obtaining 0.2moL/L, takes the sodium hydroxide of the potassium dihydrogen phosphate 50mL and 0.2moL/L of 0.2moL/L molten
Liquid 35ml mixing, is diluted to 200mL with the cold water newly boiled, the buffer solution to get pH7.2 is shaken up, as dilution；
(3) take step (1) solution, with step (2) diluted at concentration be 0.104 × 10-2mg/mL、0.208×10-3mg/
mL、0.104×10-3mg/mL、0.521×10-4The phonamiphos solution of mg/mL, while using dilution as blank control liquid；
(4) the phonamiphos solution and blank control drop for drawing 50 μ L step (3) various concentrations respectively are added in the residual test card of agriculture,
After standing 10min at room temperature, then with finger pinch 3min, after the completion of colour developing, using the colour developing card of various concentration and blank card as
Phonamiphos is tested to picture ID.
In use, the sample to be tested containing phonamiphos is added drop-wise in the residual test card of new agriculture, after colour developing, with step (4)
Multiple tests compare to picture ID, so that it is determined that content 0.521 × 10 organic phosphorus in sample to be tested-4-0.104×10- 3Within the scope of mg/mL；The sample to be tested is detected using conventional high-performance liquid chromatography simultaneously, and sample organic phosphorous content is 0.7 × 10-4Mg/mL, 0.521 × 10-4-0.104×10-3Within the scope of mg/mL, experimental result is shown, the present invention detects card can be effective
Measure the organic phosphorous content of sample to be tested.
Embodiment 2: parathion tests the preparation method to picture ID, and concrete operations are as follows:
(1) parathion standard items powder is taken, acetonitrile dissolution is added to be made into the solution of 0.128mg/mL；
(2) preparation of dilution: taking sodium hydroxide 2g, adds distilled water to make it dissolve and be settled to 500mL with distilled water and obtains
The sodium hydroxide solution of 0.1mol/L takes potassium dihydrogen phosphate 1.36g, adds 0.1mol/L sodium hydroxide 79mL, distilled water is added to dilute
The buffer solution that pH7.4 is obtained to 200mL, as dilution；
(3) take step (1) solution, with step (2) diluted at concentration be 0.128 × 10-2mg/mL、0.256×10-3mg/
mL、0.128×10-3mg/mL、0.640×10-4The parathion solution of mg/mL, while using dilution as blank control liquid；
(4) the parathion solution and blank control drop for drawing 50 μ L step (3) various concentrations respectively are added in the residual test card of agriculture,
After standing 10min at room temperature, then with finger pinch 3min, after the completion of colour developing, using the colour developing card of various concentration and blank card as
Parathion is tested to picture ID.
In use, the sample to be tested containing parathion is added drop-wise in the residual test card of new agriculture, after colour developing, with step (4)
Multiple tests compare to picture ID, so that it is determined that content 0.128 × 10 organic phosphorus in sample to be tested-3-0.256×10- 3Within the scope of mg/mL；The sample to be tested is detected using conventional high-performance liquid chromatography simultaneously, and sample organic phosphorous content is 0.2 × 10-3Mg/mL, 0.128 × 10-3-0.256×10-3Within the scope of mg/mL, experimental result is shown, the present invention detects card can be effective
Measure the organic phosphorous content of sample to be tested.
Embodiment 3: parathion-methyl tests the preparation method to picture ID, and concrete operations are as follows:
(1) parathion-methyl standard items powder is taken, acetonitrile dissolution is added to be made into the solution of 0.120mg/mL；
(2) preparation of dilution: taking dipotassium hydrogen phosphate 5.59g and potassium dihydrogen phosphate 0.41g, distilled water added to make it dissolve, and fixed
Rong Zhizhi 1000mL obtains the buffer solution of PH8.0, as dilution；
(3) take step (1) solution, with step (2) diluted at concentration be 0.120 × 10-2mg/mL、0.240×10-3mg/
mL、0.150×10-3mg/mL、0.8×10-4The parathion-methyl solution of mg/mL, while using dilution as blank control liquid；
(4) the parathion-methyl solution and blank control drop for drawing 50 μ L step (3) various concentrations respectively are added on the residual test of agriculture
On card, after standing 15min at room temperature, then with finger 3min is pinched, after the completion of colour developing, by the colour developing card and blank card of various concentration
It tests as parathion to picture ID.
In use, the sample to be tested containing parathion is added drop-wise in the residual test card of new agriculture, after colour developing, with step (4)
Multiple tests compare to picture ID, so that it is determined that content 0.8 × 10 organic phosphorus in sample to be tested-4-0.15×10-3mg/mL
In range；The sample to be tested is detected using conventional high-performance liquid chromatography simultaneously, and sample organic phosphorous content is 0.1 × 10-3mg/
ML, 0.8 × 10-4-0.15×10-3Within the scope of mg/mL, experimental result is shown, present invention detection card can effectively measure to be measured
The organic phosphorous content of sample.
Claims (2)
1. a kind of test of quick determining residues of organophosphate pesticides content is to the preparation method of picture ID, it is characterised in that: use pH 7.2-
8.0 phosphate buffer solution as diluent, will be diluted to the dissolved organic phosphorus standard items of acetonitrile concentration 0.2 ×
10-4~0.2 × 10-2Then organic phosphorus solution of various concentration within the scope of mg/mL drips organic phosphorus solution of various concentration
It is added in the residual test card of agriculture, while a diluent is added dropwise as blank control, after the residual test card colour developing of agriculture, concentration is 0.2
×10-4~0.2 × 10-2Multiple residual test cards of colour developing agriculture within the scope of mg/mL are to test to picture ID.
2. preparation method of the test of quick determining residues of organophosphate pesticides content according to claim 1 to picture ID, feature
Be: test to picture ID in use, sample to be tested is added drop-wise in the residual test card of new agriculture, after colour developing, with concentration 0.2 ×
10-4~0.2 × 10-2Multiple tests of mg/mL range compare to picture ID, so that it is determined that content organic phosphorus in sample to be tested
Value range.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910781490.6A CN110470664A (en) | 2019-08-23 | 2019-08-23 | Quickly determine preparation method of the test to picture ID of residues of organophosphate pesticides content |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910781490.6A CN110470664A (en) | 2019-08-23 | 2019-08-23 | Quickly determine preparation method of the test to picture ID of residues of organophosphate pesticides content |
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| Publication Number | Publication Date |
|---|---|
| CN110470664A true CN110470664A (en) | 2019-11-19 |
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ID=68513579
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910781490.6A Pending CN110470664A (en) | 2019-08-23 | 2019-08-23 | Quickly determine preparation method of the test to picture ID of residues of organophosphate pesticides content |
Country Status (1)
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101413895A (en) * | 2008-11-14 | 2009-04-22 | 山西大学 | Test paper for determining sulfur dioxide content in garden stuff and edible fungus fresh-keeping can |
-
2019
- 2019-08-23 CN CN201910781490.6A patent/CN110470664A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101413895A (en) * | 2008-11-14 | 2009-04-22 | 山西大学 | Test paper for determining sulfur dioxide content in garden stuff and edible fungus fresh-keeping can |
Non-Patent Citations (6)
| Title |
|---|
| 吴晓彤等: "《现代食品的安全问题及安全检测技术研究》", 31 May 2018, 中国原子能出版社 * |
| 周睿璐等: "试纸法快速检测果蔬中敌敌畏含量的研究", 《应用化工》 * |
| 曾庆祝: "《食品质量与安全检测》", 30 September 2015, 中国质检出版社 * |
| 林婵: "《食品理化检验技术》", 31 January 2019, 九州出版社 * |
| 柳州市农产品质量安全检测中心编著: "《柳州市农产品质量安全监测体系建设与运行》", 30 June 2013, 广西科学技术出版社 * |
| 王丽燕: "《生物化学实验指导》", 31 August 2017, 北京理工大学出版社 * |
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Application publication date: 20191119 |