CN111207958A - Pretreatment agent and pretreatment package for organophosphorus pesticide detection and application thereof - Google Patents
Pretreatment agent and pretreatment package for organophosphorus pesticide detection and application thereof Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The invention relates to a pretreatment agent and a pretreatment package for detecting organophosphorus pesticide and application thereof. The pretreatment agent comprises an active adsorption substance; the active adsorption substance comprises at least two of N-propyl ethylenediamine, C18, Florisil, basic alumina and Uio-66. The pretreatment agent and the pretreatment package for pesticide detection provided by the invention are used for pretreating a detection sample, so that substances (such as acid and sugar) which possibly have adverse effects on an experimental result in the sample can be removed, pigments in a dark color sample can be removed, the influence of the original color in the sample on the interpretation of the experimental result is effectively avoided, the purification process is simple, and the purification time is short.
Description
Technical Field
The invention relates to the field of chemical detection, in particular to a pretreatment agent and a pretreatment package for organophosphorus pesticide detection and application thereof.
Background
In agricultural production, the phenomena of overdose use and overdose period use of pesticides often exist due to nonstandard pesticide use. The phenomenon is found sometimes when pesticide residues in agricultural products, particularly fruits and vegetables exceed the standard, and even pesticide events caused by the pesticide residues exceeding the standard occur. The long-term use of pesticides, especially chemical pesticides, makes the level of residual pesticides in the soil very high, so that the problem of overproof pesticide residues is particularly severe.
Along with the improvement of the food safety consciousness of people, people pay more and more attention to the problem that pesticide residues of agricultural products exceed standards, and the development of pesticide residue detection methods is stronger and stronger. The traditional methods such as liquid chromatography, gas chromatography, liquid or gas chromatography tandem mass spectrometry and the like have high sensitivity, are always problems of needing professional instruments and professionals, needing complex pretreatment and having high cost and long period, are not suitable for application of field law enforcement and monitoring of a large number of samples, and are suitable for field detection and rapid pesticide detection methods for rapidly outputting detection results. However, the existing rapid detection method has the problems that the result is accurate when a standard substance is detected in a laboratory, but various false negative and false positive are generated when an actual sample is detected, and the detection result is not ideal.
When pesticide residues are rapidly detected, organic acids and saccharides in the fruit and vegetable matrix often influence the microenvironment of detection, so that deviation of detection results is caused, and especially when the pesticide residues are rapidly detected by a color development method, the color in the fruit and vegetable often causes great interference on interpretation of the detection results, so that misjudgment of the results is caused. The sample pretreatment of a common chromogenic method rapid detection kit is usually only simple shearing, extraction by adding an extracting agent, taking an upper layer solution for color development and then judging the result, and the purification process is not usually involved, which is a reason that the chromogenic method pesticide rapid detection method is difficult to be well applied in the actual environment.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a pretreatment agent and a pretreatment package for pesticide detection, which are used for pretreating a detection sample, can preferably remove substances (such as acid and sugar) which possibly have adverse effects on an experimental result in the sample, can also remove pigments in a dark sample, and effectively avoid the influence of the original color in the sample on the interpretation of the experimental result.
The invention also provides application of the pretreatment agent and the pretreatment package in the aspect of quick detection of the pesticide by a color development method.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
a pretreatment agent for organophosphorus pesticide detection, which comprises an active adsorption substance;
the active adsorbent material comprises at least two of N-propyl ethylene diamine (PSA), C18, Florisil, basic alumina and Uio-66.
Optionally, the active adsorbent species comprises at least three of N-propyl ethylene diamine (PSA), C18, florisil, basic alumina, and Uio-66.
In the present invention, C18 is octadecylsilane chemically bonded silica, 40-60 μm.
In the present invention, Uio-66 means a metal skeleton organic material which can adsorb a pigment by pi-pi interaction.
Optionally, the active adsorbent species comprises N-propyl ethylene diamine (PSA), Florisil and Uio-66.
Optionally, the mass ratio of the N-propyl ethylenediamine (PSA), the Florisil and the Uio-66 is 3-5: 5-10: 1-3.
Optionally, the active adsorbent species comprises basic alumina, C18, and Uio-66.
Optionally, the mass ratio of the basic alumina to the C18 to the Uio-66 is 7-10: 3-5: 1-3.
Optionally, the active adsorbent species comprises basic alumina, N-propyl ethylene diamine (PSA), and Uio-66.
Optionally, the mass ratio of the basic alumina to the N-propyl ethylenediamine (PSA) to the Uio-66 is 7-10: 1-3.
Optionally, the active adsorbent species comprises N-propyl ethylene diamine (PSA), C18, and Uio-66.
Optionally, the mass ratio of the N-Propylethylenediamine (PSA), the C18 and the Uio-66 is 3-5: 1-3.
Optionally, the active adsorbent species comprise basic alumina, Florisil, N-propyl ethylene diamine (PSA), C18 and Uio-66.
The mass ratio of the basic alumina to the Florisil to the N-propyl ethylenediamine (PSA) to the C18 to the Uio-66 is 8-12: 3-5: 1-3.
Optionally, the active adsorbent species comprise basic alumina, Florisil, N-propyl ethylene diamine (PSA), C18 and Uio-66.
Optionally, the basic alumina, the florisil, the N-propyl ethylenediamine (PSA), the C18, and the Uio-66 are in a mass ratio of 10:10:4:4: 2.
According to another aspect of the invention, a pretreatment package for organophosphorus pesticide detection is provided, wherein the pretreatment package comprises any one pretreatment agent for organophosphorus pesticide detection.
Optionally, the pretreatment package further comprises a salt package, a sampler, and a filter membrane.
Optionally, the sampler is a syringe.
Optionally, the salt package is selected from a sodium chloride salt package; the aperture of the filter membrane is less than or equal to 0.22 mu m.
Optionally, the pore size of the filter is 0.22 μm.
Wherein, the filter membrane can be a filter membrane for communicating water phase with organic phase so as to be better adapted to pretreatment agents of various detection kits.
According to another aspect of the invention, the application of the pretreatment package for detecting the organophosphorus pesticide in the aspect of rapid detection of the organophosphorus pesticide is provided.
Optionally, the application comprises the steps of:
a) adding a salt bag into a sample to be treated, separating, and taking supernatant;
b) adding a pretreatment agent into the supernatant obtained in the step a), fully contacting, separating, filtering, collecting filtrate, and waiting for subsequent detection.
Optionally, the ratio of the pretreatment agent to the supernatant in step b) is 30mg/mL to 50 mg/mL.
Optionally, the separation in step a) and step b) is selected from standing separation and/or centrifugation;
the method for sufficient contact in step b) is selected from shaking, shaking or vortexing.
Alternatively, the organophosphate pesticide includes malathion, dimethoate, omethoate, phorate sulfone, phorate sulfoxide, chlorpyrifos, terbufos, methidathion, diazinon, fenamiphos and dichlorvos.
Compared with the prior art, the invention has the beneficial effects that:
(1) the pretreatment agent and the pretreatment package provided by the invention are used for pretreating a detection sample, the purification process is simple, the purification time is short, and the pretreatment agent and the pretreatment package can be well applied to the rapid detection and purification process of the organophosphorus pesticide in the field monitoring process.
(2) The pretreatment agent and the pretreatment package provided by the invention are used for pretreating a detection sample, the treatment effect is good, the treated sample liquid is nearly colorless, and the interference pigment in the sample matrix can be effectively removed.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a detection spectrum of an organophosphorus pesticide sample treated by a conventional treatment method;
FIG. 2 is a detection spectrum of an organophosphorus pesticide sample treated by the pretreatment agent and the pretreatment package provided by the invention.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1 pretreatment agent
This example provides 1#～16#The pretreatment agent samples, sample numbers and compositions thereof are listed in table 1.
TABLE 1 pretreatment agent samples and their compositions
| Numbering | Composition of pretreatment agent |
| 1# | Florisil 35 mg; PSA20 mg; uio-6610mg |
| 2# | 40mg of Florisil; PSA15 mg; uio-6615mg |
| 3# | Florisil 50 mg; PSA20 mg; uio-6610mg |
| 4# | Florisil 50 mg; PAS15 mg; uio-6615mg |
| 5# | 40mg of basic alumina; c1820mg；Uio-6610mg |
| 6# | 45mg of basic alumina; c1815mg；Uio-6610mg |
| 7# | 50mg of alkaline alumina; c1820mg；Uio-6615mg |
| 8# | 50mg of alkaline alumina; c1815mg；Uio-6610mg |
| 9# | 50mg of alkaline alumina; PSA10 mg; uio-6610mg |
| 10# | 45mg of basic alumina; PSA15 mg; uio-6610mg |
| 11# | 50mg of alkaline alumina; PSA15 mg; uio-6615mg |
| 12# | PSA20mg；C1820mg；Uio-6610mg |
| 13# | PSA20mg；C1815mg；Uio-6615mg |
| 14# | PSA25mg；C1815mg；Uio-6610mg |
| 15# | PSA20mg；C1820mg；Uio-6615mg |
| 16# | 50mg of alkaline alumina; florisil 50 mg; PSA20 mg; c1820 mg; uio-6610mg |
Example 2 pretreatment package
B1 provided by the embodiment#～B16#Pretreatment packages each comprising 1 in example 1#～16#A sample of the pretreatment agent, a sodium chloride salt pack, a syringe and a 0.22 μm filter membrane which are used in combination with the respective pretreatment agents.
EXAMPLE 3 pretreatment of samples
As provided in example 2 as B1#～B16#The pretreatment package is typical, and is used for pretreating a sample to be detected, and the pretreatment package specifically comprises the following steps:
1) treating a sample according to a pretreatment method provided by the detection kit, adding a sodium chloride salt bag, standing for layering, and taking supernatant;
2) adding 1.5mL of the supernatant into a purifying agent tube filled with a pretreatment agent, fastening a tube cover, and shaking for about 30 s;
3) fixing and standing the fully shaken purification tube for layering, carefully sucking about 1mL of liquid by using an injector, removing the needle of the injector, filtering the liquid through a 0.22 mu m filter membrane, and collecting filtrate for later use;
4) and (3) carrying out color development and result interpretation on the sample filtrate collected in the step 3) according to the detection requirements of the detection kit.
It should be noted that the manual "shaking" in step 2) may be replaced by vortexing or shaking by a vortexing instrument; the "standing" in step 3) may be replaced by centrifugation with a centrifuge.
Experimental example 1 application of pretreatment Package
The samples to be detected containing 12 organophosphorus pesticide components of malathion, dimethoate, omethoate, phorate sulfone, phorate sulfoxide, chlorpyrifos, terbufos, methidathion, diazinon, fenamiphos and dichlorvos respectively adopt the traditional pretreatment method and the pretreatment bag B1 provided in the embodiment 2 of the invention#And (4) carrying out pretreatment, and detecting the treated sample.
The traditional treatment method specifically comprises the following steps:
10g of sample (accurate to 0.01g) is weighed into a 50mL plastic centrifuge tube, 10mL of acetonitrile, 6g of anhydrous sulfuric acid and 1.5g of sodium chloride are added, a centrifuge tube cover is covered, and the sample is centrifuged for 5min at the rotating speed of 5000r/min after being vigorously shaken for 2 min. 6mL of the supernatant was aspirated and added to a centrifuge tube containing 150mg of PSA and 15mg of GCB, and mixed for 1 min. Centrifuging at 5000r/min for 5min, accurately sucking 2mL supernatant into 10mL test tube, blowing nitrogen gas in 40 deg.C water bath to near dry, adding 1mL ethyl acetate for redissolving, and filtering with microporous membrane for determination.
The pretreatment package B1 provided in example 2 was used#The specific treatment method comprises the following steps:
weighing 10g of sample (accurate to 0.01g) in a 50mL plastic centrifuge tube, adding 10mL of acetonitrile and 6g of sodium chloride, covering a centrifuge tube cover, violently shaking for 3min, and centrifuging for 5min at the rotating speed of 5000 r/min. Pipette 2mL of supernatant into the column containing pretreatment bag B1#The pretreatment agent is evenly mixed in a centrifuge tube for 1min, then the centrifuge tube is centrifuged for 5min at the rotating speed of 6000r/min, and supernatant fluid is absorbed and passes through a microporous filter membrane to be measured.
The detection method and the instrument information adopted by the sample to be detected are as follows:
detecting the sample by adopting a gas chromatography-tandem mass spectrometry method, detecting a DB-5MS chromatographic column by using a gas chromatography-tandem mass spectrometry detector, and carrying out temperature programming: the initial temperature is kept at 50 ℃ for 1min, then the temperature is increased to 190 ℃ at 40 ℃/min for 1min, then the temperature is increased to 225 ℃ at 5 ℃/min for 1min, and then the temperature is increased to 290 ℃ at 40 ℃/min for 3 min. The ion monitoring mode was selected and the ion information is shown in table 2.
As a comparative example, a sample treated and tested by a conventional pretreatment method is shown in FIG. 1. Typically, the pretreatment package B1 provided in example 2 was used#The results of the measurement of the sample containing the organophosphorus pesticide component are shown in FIG. 2.
TABLE 2 Ionic information for each organophosphorus pesticide assay
| Name (R) | Quantitative ion | Qualitative ion 1 | Qualitative ion 2 |
| Malathion | 173 | 127 | 158 |
| Leguo (fruit of musical instruments) | 87 | 125 | 93 |
| Omethoate fruit | 156 | 141 | 110 |
| Phorate | 260 | 231 | 121 |
| Methylphosphine sulfoxide | 125 | 153 | 199 |
| Methylphosphine sulfone | 125 | 153 | 199 |
| Chlorpyrifos | 314 | 316 | 286 |
| Terbufos | 231 | 153 | 288 |
| Methidathion | 145 | 85 | 125 |
| Diazinon | 304 | 179 | 152 |
| Miao ethephon | 158 | 139 | 200 |
| Dichlorvos | 191 | 115 | 151 |
From the spectrum results of fig. 1 and fig. 2, it can be found that compared with the conventional method, the sample treated by the pretreatment agent and the pretreatment package provided by the present invention has more symmetrical chromatographic peak, higher response and narrower half-peak width.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The pretreatment agent for detecting the organophosphorus pesticide is characterized by comprising an active adsorption substance;
the active adsorption substance comprises at least two of N-propyl ethylenediamine, C18, Florisil, basic alumina and Uio-66.
2. The pretreatment agent for organophosphorus pesticide detection according to claim 1, wherein the active adsorption substance comprises N-propylethylenediamine, Florisil and Uio-66;
the mass ratio of the N-propyl ethylenediamine to the Florisil to the Uio-66 is 3-5: 5-10: 1-3.
3. The pretreatment agent for organophosphorus pesticide detection according to claim 1, wherein the active adsorption substance comprises basic alumina, C18 and Uio-66;
the mass ratio of the basic alumina to the C18 to the Uio-66 is 7-10: 3-5: 1-3.
4. The pretreatment agent for organophosphorus pesticide detection according to claim 1, wherein the active adsorption substance comprises basic alumina, N-propylethylenediamine and Uio-66;
the mass ratio of the alkaline alumina to the N-propyl ethylenediamine to the Uio-66 is 7-10: 1-3.
5. The pretreatment agent for organophosphorus pesticide detection according to claim 1, wherein the active adsorption substance comprises N-propylethylenediamine, C18 and Uio-66;
the mass ratio of the N-propylethylenediamine to the C18 to the Uio-66 is 3-5: 1-3.
6. The pretreatment agent for organophosphorus pesticide detection according to claim 1, wherein the active adsorption substance comprises basic alumina, florisil, N-propyl ethylenediamine, C18 and Uio-66;
the mass ratio of the basic alumina to the Florisil to the N-propyl ethylenediamine to the C18 to the Uio-66 is 8-12: 3-5: 1-3.
7. A pretreatment package for organophosphorus pesticide detection, characterized by comprising the pretreatment agent for organophosphorus pesticide detection according to any one of claims 1 to 6;
preferably, the pretreatment package further comprises a salt package, a sampler and a filter membrane;
further preferably, the sampler is a syringe;
further preferably, the salt package is selected from a sodium chloride salt package; the aperture of the filter membrane is less than or equal to 0.22 mu m.
8. The application of the pretreatment package for detecting organophosphorus pesticide disclosed by claim 7 in the aspect of rapid detection of organophosphorus pesticide.
9. The application according to claim 8, characterized in that it comprises the steps of:
a) adding a salt bag into a sample to be treated, separating, and taking supernatant;
b) adding a pretreatment agent into the supernatant obtained in the step a), fully contacting, separating, filtering, collecting filtrate, and waiting for subsequent detection;
preferably, the ratio of the pretreatment agent to the supernatant in step b) is 30 mg/mL-50 mg/mL;
preferably, the separation in step a) and step b) is selected from standing separation and/or centrifugation;
the method for sufficient contact in step b) is selected from shaking, shaking or vortexing.
10. Use according to claim 8, characterized in that the organophosphorus pesticides include malathion, dimethoate, omethoate, phorate sulfone, phorate sulfoxide, chlorpyrifos, terbufos, methidathion, diazinon, fenamiphos and dichlorvos.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113791146A (en) * | 2021-08-27 | 2021-12-14 | 浙江工业大学 | Method for detecting organic phosphate pollutants in food and sample treatment method thereof |
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