CN111982882B - Method for simultaneously and rapidly detecting carbendazim and thiophanate-methyl residues in tobacco - Google Patents
Method for simultaneously and rapidly detecting carbendazim and thiophanate-methyl residues in tobacco Download PDFInfo
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Abstract
The invention provides a method for simultaneously and rapidly detecting carbendazim and thiophanate-methyl residues in tobacco, which comprises the following steps: (1) adding an organic reagent into a tobacco sample, carrying out ultrasonic oscillation, transferring the liquid into a new centrifugal tube, adding a purifying agent, carrying out vortex oscillation and centrifugation, drying an organic layer, adding a complex solution for redissolving, and layering to obtain an upper carbendazim solution to be detected and a lower thiophanate-methyl solution to be detected; (2) and (3) uniformly mixing the solution to be detected with the agglomeration agent and the nanogold sol, detecting by using a portable Raman spectrometer, and analyzing the detected surface enhanced Raman spectrogram to obtain the detection results of the carbendazim and the thiophanate-methyl.
Description
Technical Field
The invention relates to a method for detecting pesticides carbendazim and thiophanate-methyl, in particular to a method for detecting residual carbendazim and thiophanate-methyl in tobacco by using surface-enhanced Raman spectroscopy, belonging to the field of pesticide residue analysis and detection.
Background
Both carbendazim and thiophanate-methyl belong to benzimidazoles, are bactericides with the characteristics of high efficiency, broad spectrum and low toxicity, play a role in sterilizing by interfering the formation of a spindle body in mitosis of pathogenic bacteria to influence cell division, and are widely applied to the prevention and control of plant fungal diseases in agricultural production. Thiophanate-methyl is a pesticide registered and used on tobacco and can be metabolized into carbendazim in plants. Researches show that thiophanate methyl has genotoxicity and reproductive toxicity, and the degradation or metabolite carbendazim has long residual effect period and accumulative toxicity. In view of the potential risks of wide application and dose dependence of carbendazim and thiophanate-methyl, the development of rapid detection of carbendazim and thiophanate-methyl residues is of great significance.
At present, the detection methods of carbendazim and thiophanate-methyl residues mainly comprise liquid chromatography and a mass spectrometry combined technology, an immunoassay method and the like. For example, patent 200610097540.1 and patent 201710608203.2 disclose liquid chromatography detection methods for carbendazim and thiophanate-methyl residues in vegetables and dendrobium officinale. Patent 201410486081.0 discloses a method for simultaneously detecting pesticide residues such as carbendazim and thiophanate-methyl in citrus by using a liquid chromatography-mass spectrometer. The method has the advantages of high detection sensitivity, strong specificity and the like, but complex pretreatment processes such as extraction, purification and the like are often needed, the period is long, the cost is high, expensive large-scale instruments are needed, and the method is not suitable for field rapid detection of batch samples. Patent 201710250425.1 discloses a carbendazim and thiophanate-methyl two-in-one enzyme linked immunosorbent assay kit, which has the advantages of rapidness, simplicity and the like compared with the traditional instrument analysis technology, but still needs to be further researched and improved in the aspects of obtaining high-titer and high-specificity antibodies and improving the detection sensitivity and detection limit of the method. Moreover, carbendazim and thiophanate-methyl have similar structures, and the problem of mutual interference between the carbendazim and the thiophanate-methyl is still not well solved by the conventional rapid detection method. Therefore, the method for detecting carbendazim and thiophanate-methyl, which has the advantages of strong specificity, low cost, simple and convenient operation and high detection speed, has important practical significance.
The Surface Enhanced Raman Spectroscopy (SERS) is a very effective tool for detecting intermolecular interactions and characterizing surface molecular adsorption behavior and molecular structure, has the advantages of high detection sensitivity, simple sample pretreatment, high analysis speed, small instrument volume, portability, low detection cost and the like, and is receiving more and more attention in the aspect of rapid detection of environmental pollutants, edible additives, pesticide residues and the like.
Disclosure of Invention
The invention aims to provide a method for simultaneously and rapidly detecting carbendazim and thiophanate-methyl in tobacco based on surface enhanced Raman spectroscopy.
In order to realize the aim, the invention provides a method for simultaneously and rapidly detecting carbendazim and thiophanate-methyl residues in tobacco, which comprises the following steps:
(1) adding an organic reagent into a tobacco sample, carrying out ultrasonic oscillation, transferring the liquid into a new centrifugal tube, adding a purifying agent, carrying out vortex oscillation and centrifugation, drying an organic layer, adding a complex solution for redissolving, and layering to obtain an upper carbendazim solution to be detected and a lower thiophanate-methyl solution to be detected;
wherein the organic solvent is a mixed solvent of acetonitrile and toluene in order to fully dissolve the carbendazim and the thiophanate-methyl; the composite solution is a mixed solvent of cyclohexane and pure water,
in order to remove interference of pigments, polyphenol and the like in tobacco, the purifying agent is N-propyl ethylenediamine bonded solid phase adsorbent (PSA) and anhydrous magnesium sulfate;
(2) and (3) uniformly mixing the solution to be detected with the agglomeration agent and the nanogold sol, detecting by using a portable Raman spectrometer, and analyzing the detected surface enhanced Raman spectrogram to obtain the detection results of the carbendazim and the thiophanate-methyl.
In some embodiments, in step (1), to achieve sufficient dissolution of carbendazim and thiophanate-methyl, the tobacco sample is treated in a 1: 5-20, and mixing with an organic reagent, and carrying out ultrasonic oscillation for 1-5 min. The volume ratio of the organic solvent is 5: 0.5-2.5 of a mixed solvent of acetonitrile and toluene.
In some embodiments, in order to remove interference of pigments, polyphenols and the like in tobacco, in step (1), N-propylethylenediamine bonded solid phase adsorbent (PSA) and anhydrous magnesium sulfate are used as purifying agents, the amount of the PSA is 0-0.1 g per gram of tobacco sample, the amount of the anhydrous magnesium sulfate is 0.1-1 g per gram of tobacco sample, vortex oscillation is performed for 1-3 min, and centrifugation is performed for 1-2 min at 8000-10000 r/min.
In some embodiments, in step (1), the volume ratio of the double solution is 1: 1-3 of cyclohexane and pure water mixed solvent, adding the complex solution, performing vortex oscillation for 1-3 min, and centrifuging for 1-2 min at 8000-10000 r/min to obtain a sample solution to be detected; wherein the upper layer is a carbendazim solution to be tested, and the lower layer is a thiophanate-methyl solution to be tested.
In some embodiments, in order to adjust the ionic strength of the system and obtain the optimal enhancement capability of the gold nanoparticles, in the step (2), the agglomerating agent is one or a mixture of sodium chloride, potassium carbonate, potassium bromide, potassium chloride, sodium sulfate, magnesium sulfate and potassium iodide, and preferably, the agglomerating agent used in the upper carbendazim solution is 1mol/L potassium carbonate and 1mol/L potassium bromide aqueous solution in a volume ratio of 1: 2-5, wherein the lower thiophanate-methyl solution to be detected is 0.5-1.5 mol/L sodium chloride aqueous solution as an agglomerant;
in some embodiments, in the step (2), the particle size of the nanogold sol particle is 20 to 150nm, and in order to ensure the uniformity of the size and the shape of the synthesized nanogold and the stability of the nanogold sol system and comprehensively consider the reinforcing capability of the nanogold sol in the system, the particle size of the nanogold sol particle is preferably 50 to 80 nm.
In some embodiments, in the step (2), the volume ratio of the solution to be tested, the agglomerating agent and the nanogold sol is 1: 0.1-1: 0.8 to 6; preferably, the volume ratio of the solution to be detected, the agglomerating agent and the nanogold sol is 1: 0.2-0.6: 1 to 4.
In some embodiments, in step (2), the parameters of the portable raman spectrometer are 785nm of excitation light source, 50-500 mW of excitation power, and 100-10000 ms of scanning time, preferably 500mW of excitation power and 5000ms of scanning time.
In some embodiments, in step (2), the collected surface enhanced raman spectrum of the sample is compared with the surface enhanced raman spectrum of the carbendazim and thiophanate-methyl standard, wherein the surface enhanced raman characteristic peak of the carbendazim is: 625cm-1、756cm-1、903cm-1、940cm-1、1006cm-1、1082cm-1、1224cm-1、1263cm-1(ii) a The surface enhanced Raman characteristic peak of thiophanate methyl: 605cm-1、712cm-1、961cm-1、1039cm-1、1189cm-1、1259cm-1(ii) a And judging whether the sample contains carbendazim or thiophanate-methyl according to the characteristic peak.
Compared with the existing detection method, the method for simultaneously and rapidly detecting the carbendazim and thiophanate methyl residues in the tobacco has the obvious advantage of strong specificity. The method separates carbendazim and thiophanate-methyl into different solvent layers of the same treatment solution through simple pretreatment, and combines a suitable agglomerant system and the fingerprint identification advantage of surface enhanced Raman spectroscopy, thereby realizing the specific identification of the thiophanate-methyl and the carbendazim in the rapid detection method.
In addition, the method provided by the invention has the advantages of simple pretreatment steps of the tobacco samples, convenience in operation, rapidness, high efficiency, low cost, small organic reagent dosage, no dependence on large-scale equipment and suitability for rapid screening of field batch samples.
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FIG. 1 is a solid Raman spectrum of carbendazim and surface enhanced Raman spectra of standard solutions with different concentrations, wherein a is a gold sol blank, b, c, d and e are respectively surface enhanced Raman spectra of 0.01, 0.05, 0.1 and 0.2mg/L of carbendazim standard solutions, and f is a solid Raman spectrum of carbendazim;
FIG. 2 is a solid Raman spectrum of thiophanate-methyl and surface enhanced Raman spectra of standard solutions with different concentrations, wherein a is a gold sol blank, b, c, d and e are respectively the surface enhanced Raman spectra of the thiophanate-methyl standard solutions of 0.01, 0.05, 0.1 and 0.2mg/L, and f is the solid Raman spectrum of thiophanate-methyl;
FIG. 3 is a surface enhanced Raman spectrum of a tobacco sample containing carbendazim, wherein a, b and c are respectively surface enhanced Raman spectra of a tobacco sample extract containing 0, 1 and 4mg/kg of carbendazim, and d is a surface enhanced Raman spectrum of a carbendazim standard product;
FIG. 4 is a surface enhanced Raman spectrum of a tobacco sample containing thiophanate-methyl, wherein a, b and c are respectively a surface enhanced Raman spectrum of a tobacco sample extract containing 0, 2 and 5mg/kg thiophanate-methyl, and d is a surface enhanced Raman spectrum of a thiophanate-methyl standard substance;
fig. 5 is a surface-enhanced raman spectrum of a tobacco sample containing both carbendazim and thiophanate-methyl, wherein a is a detection result of an upper layer to-be-detected liquid of a No. 1 tobacco sample, b is a detection result of an upper layer to-be-detected liquid of a No. 2 tobacco sample, c is a detection result of a lower layer to-be-detected liquid of a No. 1 tobacco sample, and d is a detection result of a lower layer to-be-detected liquid of a No. 2 tobacco sample.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the accompanying drawings and examples. It should be understood that the detailed description and specific examples, while indicating the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention
Preparation of nano gold sol
200mL of a 0.01 wt% chloroauric acid solution was boiled, and then 1.5mL of a sodium citrate solution (1 wt% concentration) was rapidly added thereto at a time to turn reddish brown about 3min, kept boiling for 30min, and cooled for use.
Raman spectrum collection of carbendazim standard product
And (3) placing the standard carbendazim solid powder on a clean glass slide, flattening, and then carrying out Raman spectrum collection on a portable Raman spectrometer to obtain a Raman spectrum shown in figure 1.
Respectively preparing carbendazim standard aqueous solution with the concentration of 0.2, 0.1, 0.05, 0.01 and 0mg/L, taking 100 mu L of standard solution, adding 50 mu L of aggregating agent (1mol/L potassium carbonate is mixed with 1mol/L potassium bromide aqueous solution according to the volume ratio of 1: 4), adding 300 mu L of gold nano sol, exciting at 785nm,the laser power is 500mW, and the scanning time is 5000ms, and the surface enhanced Raman spectrum is collected by a portable Raman spectrometer, and the result is shown in figure 1. Comparing the Raman spectrogram of carbendazim solid powder and gold sol blank, the characteristic spectral peak of carbendazim has 625cm-1、756cm-1、903cm-1、940cm-1、1006cm-1、1082cm-1、1224cm-1、1263cm-1. The result shows that the detection concentration of the detection method for the carbendazim standard solution can reach 0.01 mg/L.
Raman spectrum collection of thiophanate methyl standard product
Placing the standard thiophanate methyl solid powder on a clean glass slide, flattening, and performing Raman spectrum collection on a portable Raman spectrometer to obtain a Raman spectrum shown in figure 2.
Respectively preparing 0.2, 0.1, 0.05, 0.01 and 0mg/L thiophanate methyl standard aqueous solution, taking 200 mu L of standard solution, adding 50 mu L of agglomeration agent (1mol/L sodium chloride aqueous solution), adding 200 mu L of gold nano sol, and collecting a surface enhanced Raman spectrum by using a portable Raman spectrometer under the conditions of 785nm of exciting light, 500mW of laser power and 5000ms of scanning time, wherein the result is shown in figure 2. Comparing the Raman spectrogram of the thiophanate-methyl solid powder and the blank of gold sol, the characteristic peak of the thiophanate-methyl has 605cm-1、712cm-1、961cm-1、1039cm-1、1189cm-1、1259cm-1. The result shows that the detection concentration of the detection method for the thiophanate methyl standard solution can reach 0.01 mg/L.
Example one detection of tobacco samples containing carbendazim
Respectively weighing 0.5g of tobacco sample (the content of carbendazim is respectively 0, 1 and 4mg/kg as measured by liquid chromatography-mass spectrometry), adding 4mL of organic reagent (acetonitrile and toluene are mixed according to the proportion of 5: 1), ultrasonically oscillating for 2min, taking supernatant into a new centrifuge tube, adding 0.2g of anhydrous magnesium sulfate and 0.03g of PSA purifying agent, carrying out vortex oscillation for 2min, centrifuging for 2min at 8000r/min, taking 3mL of organic layer nitrogen for drying, adding 500 mu L of purified water and 250 mu L of cyclohexane, carrying out vortex oscillation for 2min, centrifuging for 2min at 8000r/min, and taking the upper organic layer as the liquid to be measured. Taking 100 mu L of liquid to be detected, adding 50 mu L of agglomeration agent (1mol/L potassium carbonate and 1mol/L potassium bromide aqueous solution are mixed according to the volume ratio of 1: 4), adding 300 mu L of nano gold sol, mixing uniformly, and collecting the Raman spectrum of the sample by using a portable Raman spectrometer under the conditions of 785nm of excitation light source, 500mW of laser power and 5000ms of scanning time, wherein the result is shown in figure 3.
Example II detection of tobacco samples containing thiophanate-methyl
Respectively weighing 0.5g of tobacco sample (the content of thiophanate methyl is respectively 0, 2 and 5mg/kg as measured by liquid chromatography-mass spectrometry), adding 4mL of organic reagent (acetonitrile and toluene are mixed according to the proportion of 5: 1) and ultrasonically oscillating for 2min, taking supernatant fluid to a new centrifuge tube, adding 0.25g of anhydrous magnesium sulfate and 0.04g of PSA purifying agent, carrying out vortex oscillation for 2min, centrifuging at 8000r/min for 2min, taking 3mL of organic layer nitrogen for drying, adding 500 mu L of purified water and 200 mu L of cyclohexane, carrying out vortex oscillation for 2min, centrifuging at 8000r/min for 2min, and taking the lower water layer as the liquid to be measured. And (3) adding 50 mu L of an agglomeration agent (1mol/L aqueous sodium chloride solution) into 200 mu L of the solution to be detected, adding 200 mu L of nano-gold sol, uniformly mixing, and collecting the Raman spectrum of the sample by using a portable Raman spectrometer under the conditions of 785nm of excitation light source, 500mW of laser power and 5000ms of scanning time. The results are shown in FIG. 4.
Example III detection of tobacco leaf sample containing carbendazim and thiophanate-methyl
Respectively weighing 0.5g of tobacco sample (the content of carbendazim and thiophanate-methyl in the sample No. 1 is respectively 2mg/kg and 9mg/kg measured by liquid chromatography-mass spectrometry, the content of carbendazim and thiophanate-methyl in the sample No. 2 is respectively 4mg/kg and 6mg/kg), adding 4mL of organic reagent (acetonitrile and toluene are mixed according to the proportion of 5: 1), ultrasonically oscillating for 2min, taking the supernatant into a new centrifuge tube, adding 0.3g of anhydrous magnesium sulfate and 0.03g of PSA purifying agent, spirally oscillating for 2min, centrifuging for 2min at 8000r/min, taking 3mL of organic layer nitrogen for drying, adding 500 μ L of purified water and 250 μ L of cyclohexane, spirally oscillating for 2min, centrifuging for 2min at 8000r/min, respectively processing the upper organic layer and the lower water layer according to the methods of the first embodiment and the second embodiment, detecting the thiophanate-methyl in the upper organic layer and the lower water layer, the results are shown in FIG. 5.
The above-mentioned embodiments are intended to illustrate the technical solutions and advantages of the present invention, and it should be understood that the above-mentioned embodiments are only the most preferred embodiments of the present invention, and are not intended to limit the present invention, and any modifications, additions, equivalents, etc. made within the scope of the principles of the present invention should be included in the scope of the present invention.
Claims (12)
1. A method for simultaneously and rapidly detecting carbendazim and thiophanate-methyl residues in tobacco is characterized by comprising the following steps:
(1) adding a tobacco sample into an organic solvent, carrying out ultrasonic oscillation, transferring the liquid into a new centrifugal tube, adding a purifying agent, carrying out vortex oscillation and centrifugation, drying an organic layer, adding a complex solution for redissolving, and layering to obtain an upper carbendazim solution to be detected and a lower thiophanate-methyl solution to be detected;
wherein the organic solvent is a mixed solvent of acetonitrile and toluene, the complex solution is a mixed solvent of cyclohexane and pure water,
the purifying agent is N-propyl ethylenediamine bonded solid phase adsorbent PSA and anhydrous magnesium sulfate;
(2) and (3) uniformly mixing the solution to be detected with the agglomeration agent and the nanogold sol, detecting by using a portable Raman spectrometer, and analyzing the detected surface enhanced Raman spectrogram to obtain the detection results of the carbendazim and the thiophanate-methyl.
2. The method of claim 1,
in the step (1), the tobacco sample is processed according to the proportion of 1: 5-20, and mixing with an organic solvent, and carrying out ultrasonic oscillation for 1-5 min, wherein the volume ratio of the organic solvent is 5: 0.5-2.5 of a mixed solvent of acetonitrile and toluene;
the dosage of the PSA in each gram of tobacco sample is 0-0.1 g, the dosage of the anhydrous magnesium sulfate is 0.1-1 g, the vortex oscillation is performed for 1-3 min, and the tobacco sample is centrifuged for 1-2 min at 8000-10000 r/min.
3. The method according to claim 1, wherein in the step (1), the volume ratio of the double solution is 1: 1-3 of cyclohexane and pure water mixed solvent, adding the complex solution, performing vortex oscillation for 1-3 min, and centrifuging for 1-2 min at 8000-10000 r/min to obtain a sample solution to be detected; wherein the upper layer is a carbendazim solution to be tested, and the lower layer is a thiophanate-methyl solution to be tested.
4. The method of claim 1, wherein in step (2), the agglomerating agent is one or more of sodium chloride, potassium carbonate, potassium bromide, potassium chloride, sodium sulfate, magnesium sulfate and potassium iodide.
5. The method as claimed in claim 4, wherein the agglomeration agent used in the upper carbendazim solution is 1mol/L potassium carbonate and 1mol/L potassium bromide water solution in a volume ratio of 1: 2-5, and the lower thiophanate-methyl solution to be tested is 0.5-1.5 mol/L sodium chloride aqueous solution as an agglomeration agent.
6. The method according to claim 1, wherein in the step (2), the nano gold sol particles have a particle size of 20 to 150 nm.
7. The method according to claim 6, wherein the particle size of the nano gold sol particles is 50-80 nm.
8. The method according to claim 1, wherein in the step (2), the volume ratio of the solution to be detected, the agglomerating agent and the nanogold sol is 1: 0.1-1: 0.8 to 6.
9. The method according to claim 1, wherein in the step (2), the parameters of the portable Raman spectrometer are 785nm of an excitation light source, 50-500 mW of excitation power and 100-10000 ms of scanning time.
10. The method of claim 9, wherein the excitation power is 500mw and the scan time is 5000 ms.
11. The method of claim 1, wherein in step (2), the collected surface-enhanced Raman spectrum of the sample is compared with the surface-enhanced Raman spectra of the carbendazim and the thiophanate-methyl standard, wherein the surface-enhanced Raman characteristic peaks of the carbendazim are as follows: 625cm-1、756 cm-1、903 cm-1、940 cm-1、1006 cm-1、1082 cm-1、1224 cm-1、1263 cm-1(ii) a Surface enhanced raman characteristic peaks of thiophanate methyl: 605cm-1、712 cm-1、961 cm-1、1039 cm-1、1189 cm-1、1259 cm-1(ii) a And judging whether the sample contains carbendazim or thiophanate-methyl according to the characteristic peak.
12. The method according to claim 8, wherein the volume ratio of the solution to be tested, the agglomerating agent and the nanogold sol is 1: 0.2-0.6: 1 to 4.
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