AU2021104197A4 - Method for rapid determination of total paraoxons by UV-Vis spectrometry - Google Patents

Method for rapid determination of total paraoxons by UV-Vis spectrometry Download PDF

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AU2021104197A4
AU2021104197A4 AU2021104197A AU2021104197A AU2021104197A4 AU 2021104197 A4 AU2021104197 A4 AU 2021104197A4 AU 2021104197 A AU2021104197 A AU 2021104197A AU 2021104197 A AU2021104197 A AU 2021104197A AU 2021104197 A4 AU2021104197 A4 AU 2021104197A4
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paraoxons
total
vis spectrometry
rapid
rapid determination
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AU2021104197A
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Ruichun CHEN
Hailong FU
Wenwen GONG
Bingru LI
Gang Liang
Ligang PAN
Jianhui ZHEN
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Beijing Research Center For Agricultural Standards and Testing
Shijiazhuang Technology Center For Customs District PR China
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Beijing Research Center For Agricultural Standards and Testing
Shijiazhuang Technology Center For Customs District PR China
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/33Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • 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 present invention relates to the technical field of analytical chemistry detection, and in particular to a method for rapid determination of total paraoxons by UV-Vis spectrometry, which comprises the following steps: Si. formulating a rapid hydrolysis reagent by using ultrapure water, and mixing uniformly; S2. taking and adding the mixed solution obtained from the step S Iinto a centrifugal tube, adding methylparaoxon and/or ethylparaoxon into the centrifugal tube, and mixing uniformly; S3. taking 100 L of the mixed solution obtained from the step S2, adding a proper amount of acetonitrile therein, mixing uniformly, wherein, the solution obtained thereby is recorded as a solution to be tested; and S4. formulating nitrophenol solutions respectively having a concentration different from each other, detecting nitrophenol solutions by UV-Vis spectrometry, and plotting a standard curve according to the obtained results. In the method for rapid determination of total paraoxons by UV-Vis spectrometry, the rapid hydrolysis reagent has the advantages of cheap raw materials, no pollution and being environmentally friendly, is simple to be formulated and convenient to be used, so that the hydrolysis efficiency and rate can be effectively improved. 1/2 0.06' 0.05• 0.04 0.03 0.02 0.01• 0.00' I I III 250 300 350 400 450 50m /Ilm Jn Fig. 1

Description

1/2
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0.05•
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0.03
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Fig. 1
METHOD FOR RAPID DETERMINATION OF TOTAL PARAOXONS BY UV-VIS SPECTROMETRY
Technical Field
[0001] The present invention relates to the technical field of analytical chemistry detection, and in particular to a method for rapid determination of total paraoxons by UV-Vis spectrometry.
Background
[0002] It is well-known that, the paraoxons are highly toxic organophosphorus pesticides with a broad-spectrum insecticidal effect. Meanwhile, the paraoxons residues in the environment have serious harm to environmental micro-ecology. Currently, the detection of paraoxons pesticides are performed mainly by using large-scale instruments, such as gas chromatography, gas chromatography-mass spectrometry, liquid chromatography, liquid chromatography-mass spectrometry and the like. These traditional analytical methods are the main methods for detection and quantitative analysis of pesticide residues. However, these methods still have shortcomings such as expensive instruments, high detection cost, long-time and complicated sample pretreatment, requirements for professional operators, unable to perform on-line or outdoor detection, and the like.
[0003] Compared with the above chromatographic methods, UV-Vis spectrometry has the advantages of low cost, simple operation, high accuracy and good reproducibility, and thus it can be widely applied in various fields. However, since the UV-Vis absorption peak of the paraoxons overlap with those of other pesticides, it is difficult to achieve specific screening and detection by the UV-Vis method.
Summary
(I) Technical problem to be solved
[0004] In view of the shortcomings of the prior art, the present invention provides a method for rapid determination of total paraoxons by UV-Vis spectrometry, such that the time for detecting is shorten, and the detection sensitivity and efficiency are improved.
(II) Technical Solutions
[0005] In order to achieve the above objective, the present invention provides the following technical solutions: a method for rapid determination of total paraoxons by UV-Vis spectrometry, including the following steps: Si. formulating a rapid hydrolysis reagent by using ultrapure water, and mixing uniformly; S2. taking and adding the mixed solution obtained from the step S Iinto a centrifugal tube, adding methylparaoxon and/or ethylparaoxon into the centrifugal tube, and mixing uniformly; S3. taking 100 L of the mixed solution obtained from the step S2, adding a proper amount of acetonitrile therein, mixing uniformly, wherein, the solution obtained thereby is recorded as a solution to be tested; S4. formulating nitrophenol solutions respectively having a concentration different from each other, detecting nitrophenol solutions by UV-Vis spectrometry, and plotting a standard curve according to the obtained results; S5. detecting the solution to be tested of the step S3 by UV-Vis spectrometry in the same batch, and determining the concentration of nitrophenol in the solution to be tested according to the standard curve plotted in the step S4; and S6. calculating the total concentration of methylparaoxon and ethylparaoxon according to the concentration of the hydrolysate nitrophenol based on the 1:1 quantitative relationship between nitrophenol and paraoxon.
[0006] Preferably, the rapid hydrolysis reagent includes one or a mixture of any one of potassium chloride, sodium phosphate, sodium acetate, sodium hydroxide, sodium citrate, sodium carbonate, magnesium sulfate and ammonium hydroxide.
[0007] Preferably, the pH of the rapid hydrolysis reagent is 6-14.
[0008] Further preferably, the pH of the rapid hydrolysis reagent is greater than 12.
[0009] Preferably, the time for the mixing and stirring in the step S2 is 5-45 min.
[0010] Preferably, the amount of acetonitrile in the step S3 is between 0-25% in proportion.
[0011] Further preferably, the amount of acetonitrile in the step S3 is between 0-10% in proportion.
(III) Beneficial Effects
[0012] Compared with the prior art, the present invention provides a method for rapid determination of total paraoxons by UV-Vis spectrometry, wherein the beneficial effects thereof are as follows:
[0013] In the method for rapid determination of total paraoxons by UV-Vis spectrometry, the rapid hydrolysis reagent has the advantages of cheap raw materials, no pollution and being environmentally friendly, is simple to be formulated and convenient to be used, so that the hydrolysis efficiency and rate can be effectively improved. In addition, the hydrolysis reagent in the present invention has the characteristic of non-toxicity, which is of great significance for the edible safety of agricultural products when a reagent suitable for cleaning agricultural products such as fruits and vegetables is prepared as needed so as to remove possibly-existed pesticide residues.
Brief Description of the Drawings
[0014] FIG. 1 shows the UV-Vis spectrum of 1 ppm of 4-MP inNaOH solution atpH 11; and
[0015] FIG. 2 shows the UV-Vis spectrum of 250 ppb of 4-NP inNaOH solution atpH 11.
Detailed Description
[0016] In the following text, the technical solutions in examples of the present invention will be described clearly and completely with reference to the examples of the present invention. Apparently, the examples as described below are merely a part rather than all of the examples of the present invention. All other examples obtained by a person of ordinary skill in the art based on the examples of the present invention without creative efforts shall fall within the protection scope of the present invention.
[0017] A method for rapid determination of total paraoxons by UV-Vis spectrometry comprises the following steps: Si. formulating a rapid hydrolysis reagent by using ultrapure water, and mixing uniformly; S2. taking and adding the mixed solution obtained from the step S Iinto a centrifugal tube, adding methylparaoxon and/or ethylparaoxon into the centrifugal tube, and mixing uniformly; S3. taking 100 L of the mixed solution obtained from the step S2, adding a proper amount of acetonitrile therein, and mixing uniformly, wherein, the solution obtained thereby is recorded as a solution to be tested; S4. formulating nitrophenol solutions respectively having a concentration different from each other, detecting nitrophenol solutions by UV-Vis spectrometry, and plotting a standard curve according to the obtained results; S5. detecting the solution to be tested of the step S3 by UV-Vis spectrometry in the same batch, and determining the concentration of nitrophenol in the solution to be tested according to the standard curve plotted in the step S4; and S6. calculating the total concentration of methylparaoxon and ethylparaoxon according to the concentration of the hydrolysate nitrophenol based on the 1:1 quantitative relationship between nitrophenol and paraoxon.
[0018] Preferably, the rapid hydrolysis reagent includes one or a mixture of anyone of potassium chloride, sodium phosphate, sodium acetate, sodium hydroxide, sodium citrate, sodium carbonate, magnesium sulfate and ammonium hydroxide.
[0019] The pH of the rapid hydrolysis reagent is adjusted such that the pH of the rapid hydrolysis reagent is 12-14.
[0020] The time for the mixing and stirring in the step S2 is 5-45 min.
[0021] The proportion of acetonitrile in the step S3 is between 0-10%.
[0022] Example 1
[0023] Formulation of a rapid hydrolysis reagent: 40 mg of sodium hydroxide, 5 mg of sodium sulfate and 7 mg of potassium chloride were weighed, then dissolved in ultrapure water, and then the volume of the obtained solution was adjusted to 10 ml, so as to obtain the rapid hydrolysis reagent. The rapid hydrolysis reagent was mixed uniformly for later use.
[0024] Example 2
[0025] The research for the hydrolysis behavior of methylparaoxon and ethylparaoxon was performed by using the rapid hydrolysis reagent formulated in Example 1. 1,000 nM methylparaoxon solution and 1,000 nM ethylparaoxon solution were respectively formulated by using the rapid hydrolysis reagent. After mixed uniformly by vortex, 100 L of the solutions were respectively taken at different reaction time and detected by UV-Vis spectrometry. The results were shown in Table 1.
Table 1 The paraoxon concentrations in the hydrolysis system over time
Time/min Paraoxons 0 1 2 10 30 Methylparaoxon 1000 352.5 128.8 34.8 24.9 /nM Ethylparaoxon 1000 993.5 984.1 544.85 104.5 /nM
[0026] It can be seen from the results that the rapid hydrolysis reagent had a significant effect on the hydrolysis of methylparaoxon and ethylparaoxon, wherein the concentrations of paraoxons in the system were decreased significantly with the extension of the reaction time. After 30 min of the reaction, 90% of both methylparaoxon and ethylparaoxon were hydrolyzed.
[0027] Test Example 3
[0028] The research for hydrolysis behavior of various pesticide systems was performed by using the rapid hydrolysis reagent formulated in Example 1. Sampling and detecting were performed according to the method in Example 2. The results of Abs detection by UV-Vis spectrometry were shown in Table 2.
Table 2 The UV-Vis (400 nm) results of different pesticides in the hydrolysis systems
Pesticides Methylparaoxon Acetamiprid Tsumacide Diazinon Profenofos Malathion
Abs 0.076 0.0001 0.0001 0.0001 0.0001 0.0001
[0029] It can be seen from the result that after the hydrolysis of methylparaoxon, acetamiprid, tsumacide, diazinon, profenofos and malathion were respectively performed for min by using the rapid hydrolysis reagent, the value of Abs in the hydrolysis system of methylparaoxon was the highest, while the values of Abs in other systems were very low. It is indicated that the UV-Vis spectrometry could be used for specific quantitative analysis of methylparaoxon.
[0030] Test Example 4
[0031] The research for hydrolysis of methylparaoxon and ethylparaoxon was performed by using the rapid hydrolysis reagent formulated in Example 1.
[0032] A solution mixture of methylparaoxon and ethylparaoxon was prepared by using the rapid hydrolysis reagent. The solution mixture was stirred by vortex and then heated for 30 min. 100 L of the solution mixture was taken and detected by UV-Vis spectrometry. The detection results and the recovery efficiency of p-nitrophenol were shown in Table 3.
Table 3 Recoveries of paraoxons determined by p-nitrophenol measurement
ParaoxonlnM P-nitrophenol Recovery Methylparaoxon/nM Ethylparaoxon/nM /nM efficiency
50 50 100.1 100.1%
100 100 183.8 91.9%
[0033] In view of the above, in the method for rapid determination of total paraoxons by UV-Vis spectrometry, the mixture system of methylparaoxon and ethylparaoxon was hydrolyzed by using the rapid hydrolysis reagent, and the recovery efficiencies are greater than 90%. Therefore, it is indicated that the UV-Vis methods could be used for determining the total amount of paraoxons.
[0034] Although embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principle and spirit of the present invention, and the scope of the present invention is defined by the appended claims and the equivalents thereof.

Claims (7)

CLAIMS:
1. A method for rapid determination of total paraoxons by UV-Vis spectrometry, comprising the following steps: Si. formulating a rapid hydrolysis reagent by using ultrapure water, and mixing uniformly; S2. taking and adding the mixed solution obtained from the step S Iinto a centrifugal tube, adding methylparaoxon and/or ethylparaoxon into the centrifugal tube, and mixing uniformly; S3. taking 100 L of the mixed solution obtained from the step S2, adding a proper amount of acetonitrile therein, and mixing uniformly, wherein, the solution obtained thereby is recorded as a solution to be tested; S4. formulating nitrophenol solutions respectively having a concentration different from each other, detecting nitrophenol solutions by UV-Vis spectrometry, and plotting a standard curve according to the obtained results; S5. detecting the solution to be tested in the step S3 by UV-Vis spectrometry in the same batch, and determining the concentration of nitrophenol in the solution to be tested according to the standard curve plotted in the step S4; and S6. calculating the total concentration of methylparaoxon and ethylparaoxon according to the concentration of the hydrolysate nitrophenol based on the 1:1 quantitative relationship between nitrophenol and paraoxon.
2. The method for rapid determination of total paraoxons by UV-Vis spectrometry according to claim 1, wherein the rapid hydrolysis reagent comprises one or a mixture of any one of potassium chloride, sodium phosphate, sodium acetate, sodium hydroxide, sodium citrate, sodium carbonate, magnesium sulfate and ammonium hydroxide.
3. The method for rapid determination of total paraoxons by UV-Vis spectrometry according to claim 1, wherein the pH of the rapid hydrolysis reagent is 6-14.
4. The method for rapid determination of total paraoxons by UV-Vis spectrometry according to claim 3, wherein the pH of the rapid hydrolysis reagent is greater than 12.
5. The method for rapid determination of total paraoxons by UV-Vis spectrometry according to claim 1, wherein the time for the mixing and stirring in the step S2 is 5-45 min.
6. The method for rapid determination of total paraoxons by UV-Vis spectrometry according to claim 1, wherein the amount of acetonitrile in the step S3 is between 0-25% in proportion.
7. The method for rapid determination of total paraoxons by UV-Vis spectrometry according to claim 6, wherein the amount of acetonitrile in the step S3 is between 0-10% in proportion.
AU2021104197A 2021-06-28 2021-07-15 Method for rapid determination of total paraoxons by UV-Vis spectrometry Ceased AU2021104197A4 (en)

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Cited By (1)

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CN113466162A (en) * 2021-06-28 2021-10-01 北京农业质量标准与检测技术研究中心 Rapid detection method of total phosphorus paraoxonate by ultraviolet spectrophotometry

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5846753A (en) * 1995-05-30 1998-12-08 The United States Of America As Represented By The Secretary Of The Army Chemiluminescence-based method for rapid and sensitive in-situ detection of organophosphorus compounds and metal ions
US6242186B1 (en) * 1999-06-01 2001-06-05 Oy Jurilab Ltd. Method for detecting a risk of cancer and coronary heart disease and kit therefor
CN101942062B (en) * 2010-08-09 2013-07-17 南开大学 Surface imprinted polymer for catalyzing degradation of organophosphorus pesticide and preparation method thereof
CN103343159A (en) * 2013-07-22 2013-10-09 上海润鸿生物科技有限公司 PON-1 (paraoxonase-1) activity detection kit and detection method for same
CN106117470B (en) * 2016-06-29 2018-05-08 陕西师范大学 The synthetic method of polymer microballoon functional graphene oxide and its application of catalytic degradation organophosphor
CN105928940A (en) * 2016-07-11 2016-09-07 苏州大学 Pesticide residue detection method and detection kit
CN108486024B (en) * 2018-03-20 2020-12-11 上海交通大学 Method for detecting organophosphorus pesticide by using sensing system based on flora
CN108587990B (en) * 2018-04-12 2020-10-09 中国科学院南海海洋研究所 Organophosphorus degradation active nano-particles and preparation method and application thereof
CN109270061B (en) * 2018-10-31 2022-01-11 青岛农业大学 Device for rapidly detecting and degrading organophosphorus pesticide and application
CN113466162A (en) * 2021-06-28 2021-10-01 北京农业质量标准与检测技术研究中心 Rapid detection method of total phosphorus paraoxonate by ultraviolet spectrophotometry

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CN113466162A (en) * 2021-06-28 2021-10-01 北京农业质量标准与检测技术研究中心 Rapid detection method of total phosphorus paraoxonate by ultraviolet spectrophotometry

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