CN110763533A - Pretreatment method suitable for detecting pesticide residues in tobacco by Raman spectrum - Google Patents
Pretreatment method suitable for detecting pesticide residues in tobacco by Raman spectrum Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/405—Concentrating samples by adsorption or absorption
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- 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
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Abstract
The invention relates to a pretreatment method suitable for detecting pesticide residues in tobacco by Raman spectroscopy, which is characterized in that an organic solvent with low toxicity and strong polarity and water are selected as an extracting agent, a hydrophilic functionalized hollow nano carbon material is prepared as a purifying agent, the preparation can be completed only by simple mixing and centrifuging processes, and a surface enhanced nano reagent is combined, so that the pretreatment method is particularly suitable for detecting the pesticide residues in the tobacco sample by Raman spectroscopy. The method reduces the dosage and toxicity of the extraction reagent, improves the purification effect of the tobacco sample, and obviously increases the detection limit and accuracy of Raman detection. Meanwhile, the method is simple to operate, the material and labor cost is reduced, and the pretreatment time is greatly shortened.
Description
Technical Field
The invention belongs to the technical field of pesticide residue detection, and particularly relates to a pretreatment method suitable for detecting pesticide residues in tobacco by Raman spectroscopy.
Background
In the process of growing tobacco leaves and storing tobacco products, diseases, insects and weeds are often damaged, and in order to not affect the quality of the tobacco leaves, pesticide is inevitably used, so that pesticide residues in the tobacco products are caused. On one hand, the pesticide residue of the tobacco is directly applied to the tobacco in a spraying mode, the pesticide adhered to the leaf surface of the tobacco enters the juice of the tobacco plant through absorption and dispersion, and particularly, the pesticide residue is not applied properly, if the tobacco leaves are applied before being harvested, and the pesticide residue is applied for many times in large concentration and large dose, the excessive pesticide residue in the tobacco leaves is more easily caused; on the other hand, the pesticide residue in the environment also affects the tobacco, particularly, the soil, irrigation water and the atmosphere, and the pesticide residue in the environment also pollutes the tobacco to cause the pesticide residue of the tobacco.
The detection requirement of pesticide residues in tobacco is high, the laboratory methods such as chromatography, mass spectrometry and the like are complex to operate and long in detection time, and the detection of a large number of tobacco samples cannot be rapidly completed. In recent years, the rapid detection technology is rapidly developed, the Raman spectrum technology used for pesticide residue detection is a current popular research field, the detection is mainly realized by the surface enhanced Raman technology, the detection speed is high, and the sensitivity is high. In actual detection, the detection effect depends on the performance of the instrument on one hand and also depends on the pretreatment mode of the tobacco sample on the other hand. At present, the pretreatment of pesticide residues mainly comprises methods such as liquid-liquid extraction, solid-phase extraction, QuEChERS and the like. A large amount of organic reagents are needed for liquid-liquid extraction, and the recovery rate is low; the solid phase extraction method has high recovery rate, but the operation steps are complex and the use cost is high. At present, the most widely used pretreatment method for pesticide residues in rapid detection is the QuEChERS method, which basically comprises the following steps: 1) crushing and homogenizing a sample; 2) adding acetonitrile, anhydrous magnesium sulfate, sodium citrate, etc. to extract, centrifugate, and remove water; 3) adding adsorbent such as ethylenediamine-N-Propyl Silane (PSA) and GCB into the supernatant, and centrifuging to remove impurities. Compared with other sample pretreatment methods, the method reduces the reagent dosage and operation time, but the pretreatment speed is still limited by operations such as multi-step sample adding, centrifugation and the like. Therefore, a pretreatment method suitable for raman spectrum detection, with good extraction and purification effects, simple operation and high speed is needed.
Disclosure of Invention
In order to solve the technical problems, the invention provides a pretreatment method suitable for detecting pesticide residues in tobacco by Raman spectrum, which specifically comprises the following steps:
a pretreatment method suitable for detecting pesticide residues in tobacco by Raman spectrum is realized by the following steps:
(1) crushing a tobacco sample, taking a powdery sample, adding a low-toxicity and strong-polarity organic solvent and water, uniformly mixing, and centrifuging to obtain a supernatant;
(2) adding the extracting solution into a functionalized hollow nano carbon material (f-HCN), uniformly mixing, standing for layering, collecting supernatant, and detecting and analyzing;
(3) and mixing the solution to be detected with the surface enhanced nano gold/silver solvent, and detecting by using a portable Raman spectrometer.
Preferably, the sampling amount of the tobacco powder sample to be detected in the step (1) is 0.5-2.5 g, and the volume of the low-toxicity and high-polarity extracting agent added is 1.5-10 ml based on the mass of the tobacco sample to be detected.
Preferably, the extractant is a mixed solution of an organic solvent and water, wherein the organic solvent is a low-toxicity and strong-polarity organic solvent which can be one or more of ethanol, dimethyl sulfoxide, acetone and ethylene glycol, and the volume ratio of the organic solvent to the water is 1: 2-9.
Preferably, the preparation method and characteristics of the functionalized hollow nano carbon material in the step (2) are as follows:
(1) taking magnesium oxide as a template and benzene as a carbon material precursor at 600-1000 deg.CoC, synthesizing a nano carbon material with a large specific surface area and a hollow square hole shape at a high temperature, wherein the aperture is uniform and is concentrated between 10 nm and 45 nm;
(2) adding the nano carbon material into an inorganic acid solution at a temperature of 45-70 DEG CoC, heating for 2-5 hours, washing for a plurality of times by using deionized water, and drying for more than 8 hours by using an oven; the obtained nano carbon material contains rich oxygen-containing functional groups.
Preferably, the inorganic acid solution in the step (2) may be one or two of nitric acid and sulfuric acid, and the concentration is 1-10 mol/L.
Preferably, the inorganic acid solution in the step (2) is a 6mol/L nitric acid solution.
Preferably, the amount of the extracting solution added in the step (2) is 0.8-2 mL, and the amount of the nanocarbon material used is 20-60 mg based on the volume of the extracting solution.
Preferably, the solution to be detected in the step (3) and the nano gold/silver enhancing reagent are mixed in a volume ratio of 1: 0.5-20.
Preferably, the portable raman spectrometer can use any light source; the single-frequency output power is less than or equal to 500mw, the spacing is less than or equal to 1nm, the line width is less than or equal to 0.06nm, and the spectrum range is as follows: 180 and 2800cm-1And the Raman spectrum scanning time for collecting the sample is 3-50 seconds.
Compared with the prior art, the invention has the following advantages: (1) the pesticide extraction agent used in the method is a mixture of an organic reagent with low toxicity and high polarity and water, the dosage of the organic reagent is small, and compared with solvents with high toxicity such as acetonitrile, toluene and the like used in most pesticide residue detection methods, the harm to human bodies and environment is obviously reduced, but the pesticide residue in the sample can be effectively extracted from the tobacco sample; meanwhile, the extractant contains a large proportion of water, and the surface-enhanced nano gold/silver reagent is an aqueous solvent, so that the extractant used in the method can be better combined with the Raman-enhanced reagent, and the detection limit is obviously improved.
(2) The invention uses functional group hollow hole carbon nanometer material as purifying agent, the square hole structure with uniform aperture makes carbon material have high specific surface area and specific surface area utilization ratio, the material has good impurity adsorption capacity, at the same time, strong acid with special condition is used to process surface functional group, the material surface has abundant and proper amount of hydroxyl, carboxyl and other oxygen-containing functional group, increases hydrophilicity and wetting quality, avoids excessive adsorption to pesticide caused by excessive oxygen-containing functional group. Therefore, the method is particularly suitable for the aqueous extractant used in the method, so that the purifying agent used in the method has excellent purifying effect and is particularly suitable for the pretreatment application of Raman technology.
(3) The extraction agent and the purifying agent have simple components, achieve better purifying effect than the conventional QuEChERS method only by using few materials, have good detection accuracy, have great cost advantage compared with most other methods, are convenient to carry, and are suitable for rapid detection on site.
(4) The method has the advantages of simple operation steps, no need of pH adjustment, no need of adding various reagents, no need of freezing in the extraction process, shortened steps and manpower for detecting the pesticide in the tobacco by the conventional method, and improved detection efficiency.
Drawings
FIG. 1: transmission electron microscopy of functionalized hollow nanocarbon material (f-HCN).
FIG. 2: and (5) pigment removal effect graphs of different purifying materials.
FIG. 3: raman spectra of acetamiprid-labeled tobacco samples treated by different purification materials.
FIG. 4: the Raman spectrogram of the tobacco sample with different standard adding concentrations of triazolone.
FIG. 5: and (3) Raman spectrograms of tobacco samples with different standard adding concentrations of chlorpyrifos.
FIG. 6: and Raman spectrograms of tobacco samples with different standard adding concentrations of carbendazim.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1 extraction reagent and raman detection technique applicability experiments are detailed below.
The commercially available methyl parathion standard is purchased, acetonitrile, toluene, acetonitrile-toluene (2: 1), ethanol-water (1: 2), acetone-water (1: 4) and dimethyl sulfoxide-water (1: 9) are respectively selected as solvents, and the concentrations of the prepared methyl parathion standard solution are 0.5mg/L, 0.1mg/L, 0.05mg/L and 0.01 mg/L.
The portable Raman spectrometer has a light source of 785nm, an output power of 450mw, a spacing of less than or equal to 1nm, a line width of less than or equal to 0.06nm, and a spectral range: 180 and 2800cm-1The raman spectrum scan time for the collected sample was 3 seconds. And sequentially adding 40 mu L of standard solution and 150 mu L of gold nano sol into the sample bottle, and uniformly mixing to perform Raman spectrometer determination.
The result shows that the detection limit of toluene as a solvent is 0.5mg/L, the detection limit is highest, the detection limit of acetonitrile and acetonitrile-toluene (2: 1) is 0.1mg/L, and the detection limit of ethanol-water (1: 2), acetone-water (1: 4) and dimethyl sulfoxide-water (1: 9) as solvents is lowest and can reach 0.01 mg/L; it is seen that when a mixture of a highly polar organic solvent and water is used as a solvent, the binding property with the surface-enhancing reagent is better, and a more excellent detection limit can be obtained.
Example 2. hollow nanocarbon material purification effect experiment, the details are as follows.
5g of magnesium carbonate is intensively piled in a tube furnace and heated to 800 ℃ under the protection of Ar gasoAnd C, decomposing the magnesium carbonate into a magnesium oxide template. 2mL of benzene precursor was injected into the furnace tube by a syringe pump and reacted at the deposition temperature for 30 min. Stopping heating until the temperature of the tube furnace is reduced to 100 DEGoTaking out the deposition product after C is less than C to obtain a hollow nano carbon material with uniform aperture and centralized aperture size of 15-35 nm; adding the nano carbon material into 6mol/L nitric acid solution at 65 DEGoAnd C, heating for 2 hours, washing for 3 times by using deionized water, and drying in an oven for 12 hours to obtain f-HCN.
Taking 2.5g of tobacco, crushing the tobacco sample, adding 10mL of ethanol-water (1: 4) solvent, and adding an acetamiprid standard substance to ensure that the concentration of the acetamiprid in the tobacco sample to be detected is 1 mg/L; vortex and mix for 1min, centrifuge for 30s at 4000 r/min, collect the supernatant. GCB, PSA, GCB + PSA + C18 (1: 1: 1) and f-HCN are respectively used as purifying agents, 30mg of the purifying agents are added into 1ml of supernatant, the mixture is shaken and evenly mixed, then the mixture is kept stand and layered, and the supernatant is to be detected. The measurement was performed under the same raman spectroscopic conditions as in example 1.
The results show that the infiltration effect of the f-HCN material and water is the best, and the pigment removal capacity f-HCN is more than GCB + PSA + C18 (1: 1: 1). apprxeq.GCB > PSA. In the acetamiprid labeling experiment result, the acetamiprid Raman characteristic peak intensity f-HCN is more than GCB + PSA + C18 (1: 1: 1) > GCB is more than PSA, which indicates that the purifying agent used by the method is more suitable for Raman spectrum detection.
Example 3 determination of triazolone residue in tobacco.
5g of magnesium carbonate is intensively piled in a tube furnace and heated to 600 ℃ under the protection of Ar gasoAnd C, decomposing the magnesium carbonate into a magnesium oxide template. 2mL of benzene precursor was injected into the furnace tube by a syringe pump and reacted at the deposition temperature for 30 min. Stopping heating until the temperature of the tube furnace is reduced to 100 DEGoTaking out the deposition product after C is less than C to obtain a hollow nano carbon material with uniform aperture and the aperture size concentrated between 10 nm and 35 nm; adding the nano carbon material into 3mol/L nitric acid solution at 65 DEGoAnd C, heating for 2 hours, washing for 3 times by using deionized water, and drying in an oven for 8 hours to obtain f-HCN.
Taking 0.5g of tobacco, crushing the tobacco sample, adding 1.5mL of acetone-water (1: 4) solvent, and adding the triazolone standard substance to ensure that the concentration of the triazolone is 5, 2, 1 and 0.5 mg/kg; vortex and mix evenly for 1min, centrifuge for 30s at 4000 r/min, take 0.8mL supernatant and add 20mg f-HCN, shake and mix evenly, and then stand and stratify, the supernatant is to be measured. The measurements were performed using the same raman spectrometer parameters as in example 1, and the raman spectrum scan time for the collected sample was 10 seconds.
The result shows that the method can well detect the residual triazolone in the tobacco, meet the national limit requirement and reach the detection limit of 1 mg/kg.
Example 4. determination of Chlorpyrifos residue in tobacco.
5g of magnesium carbonate is intensively piled up in a tube furnace and heated to 1000 ℃ under the protection of Ar gasoAnd C, decomposing the magnesium carbonate into a magnesium oxide template. 2mL of benzene precursor was injected into the furnace tube by a syringe pump and reacted at the deposition temperature for 30 min. Stopping heating until the temperature of the tube furnace is reduced to 100 DEGoTaking out the deposition product after C is less than C to obtain a hollow nano carbon material with uniform aperture and centralized aperture size of 15-45 nm; adding the nano carbon material into 3mol/L nitric acid solution at 65 DEGoAnd C, heating for 5 hours, washing for 3 times by using deionized water, and drying in an oven for 12 hours to obtain f-HCN.
1g of tobacco is taken and crushed, 3mL of dimethyl sulfoxide-water (1: 9) solvent is added, and a chlorpyrifos standard substance is added to ensure that the concentration of the chlorpyrifos is 2, 1, 0.5 and 0.2 mg/kg; and (3) uniformly mixing by vortex for 1min, centrifuging for 30s at 4000 r/min, adding 40mg f-HCN into 1mL of supernatant, uniformly mixing by oscillation, standing for layering, and measuring the supernatant. The measurement was performed under the same raman spectroscopic conditions as in example 3.
The result shows that the method can well detect the chlorpyrifos residue in the tobacco, meet the national limit requirement and reach the detection limit of 0.5 mg/kg.
Example 5. determination of carbendazim residue in tobacco.
Preparing f-HCN under the same conditions as in example 2, taking 2g of a pulverized tobacco sample, adding 4mL of glycol-water (1: 5) solvent, and adding a carbendazim standard substance to ensure that the concentration of the carbendazim is 2, 1, 0.5 and 0.2mg/kg mg/kg; vortex and mix evenly for 1min, centrifuge for 30s at 4000 r/min, take 1.5mL supernatant and add 60mg f-HCN, shake and mix evenly, and then stand and stratify, the supernatant is to be measured. The measurement was performed under the same raman spectroscopic conditions as in example 3.
The result shows that the method can well detect the carbendazim residue in the tobacco, meet the national limit requirement and reach the detection limit of 0.5 mg/kg.
Example 6. experiment compared to QuEChERS method.
And (2) detecting a tobacco sample by taking a QuEChERS method (according to the standard of YQ/T47.1-2014 tobacco and determination methods of various pesticide residues in tobacco products) as pretreatment:
1) extraction: weighing 2g of sample into a 50 mL centrifuge tube with a cover, adding 10mL of water, shaking the centrifuge tube by hand until the sample is fully mixed with the water, and centrifuging for 2min at 4000 r/min. 10mL of acetonitrile was removed from each tube and placed on a vortex mixer shaker at 2000r/min for 2 min. Freezing and storing the centrifugal tube at (-18 ℃ to-20 ℃) for 10min, and taking out. 5mL of toluene, 4 g of anhydrous magnesium sulfate, 1g of sodium chloride, 1g of sodium citrate and 0.5g of disodium hydrogen citrate are respectively added into a centrifuge tube, the centrifuge tube is immediately held by a hand to be vigorously shaken to prevent caking, then the centrifuge tube is placed on a vortex mixing and shaking instrument to be shaken for 2min at the speed of 2000r/min, and then the centrifuge tube is centrifuged for 2min at the speed of 4000 r/min. Collecting the supernatant for later use.
2) Purifying: transferring 1.5mL of sample extract supernatant into a 2mL centrifuge tube, adding 150 mg of anhydrous magnesium sulfate and 50 mg of N-propyl ethylenediamine bonded solid phase adsorbent (PSA), oscillating on a vortex mixing oscillator at a speed of 2000r/min for 2min, centrifuging at 4000 r/min for 1min, collecting supernatant, and detecting for analysis. The measurement was performed under the same Raman spectrum conditions as in examples 3 to 5.
The samples to be detected after the labeling are detected respectively according to the example 4 and the QuEChERS comparison method, the method detection limits of different pesticides are determined, and each pesticide is subjected to a labeling experiment with the detection limit concentrations of 50 samples and blank samples, and the specific results are as follows:
it can be seen that the method of the present invention has a lower detection limit and higher accuracy. Meanwhile, the sample processing speeds of the two methods are counted, 50 samples are taken as a group to be processed simultaneously, the method provided by the patent can complete the processing of all samples only in 60min, the QuEChERS method needs 180min which is 3 times of the method, and the method greatly shortens the pretreatment time.
The above examples are illustrative of the method of using the present invention, but the protection of the present invention is not limited to the use of the examples, and the modifications of the nature of the natural extension performed by the skilled person in the art according to the present invention also belong to the protection scope of the present invention.
Claims (8)
1. A pretreatment method suitable for detecting pesticide residues in tobacco by Raman spectrum is characterized by comprising the following steps:
(1) crushing a tobacco sample, taking a powdery sample, adding a low-toxicity and strong-polarity organic solvent and water, uniformly mixing, and centrifuging to obtain a supernatant;
(2) adding the extracting solution into a functionalized hollow nano carbon material (f-HCN), uniformly mixing, standing for layering, collecting supernatant, and detecting and analyzing;
(3) and mixing the solution to be detected with the surface enhanced nano gold/silver solvent, and detecting by using a portable Raman spectrometer.
2. The pretreatment method for detecting the pesticide residue in the tobacco by the Raman spectrum according to claim 1, wherein the sampling amount of the tobacco powder sample to be detected in the step (1) is 0.5-2.5 g, and the volume of the low-toxicity and high-polarity extractant added is 1.5-10 ml based on the mass of the tobacco sample to be detected.
3. The pretreatment method suitable for detecting the pesticide residue in the tobacco by the Raman spectrum according to claim 1 or 2, wherein the extracting agent is a mixed solution of an organic solvent and water, wherein the organic solvent is a low-toxicity and strong-polarity organic solvent which can be one or more of ethanol, dimethyl sulfoxide, acetone and ethylene glycol, and the volume ratio of the organic solvent to the water is 1: 2-9.
4. The pretreatment method suitable for detecting pesticide residues in tobacco by Raman spectroscopy as claimed in claim 1, wherein the preparation method and characteristics of the functionalized hollow nano carbon material in step (2) are as follows:
(1) using magnesium oxide as template and benzene as carbon material precursor in600~1000oC, synthesizing a nano carbon material with a large specific surface area and a hollow square hole shape at a high temperature, wherein the aperture is uniform and is concentrated between 10 nm and 45 nm;
(2) adding the nano carbon material into an inorganic acid solution at a temperature of 45-70 DEG CoC, heating for 2-5 hours, washing for a plurality of times by using deionized water, and drying for more than 8 hours by using an oven; the obtained nano carbon material contains rich oxygen-containing functional groups.
5. The pretreatment method for detecting the pesticide residue in the tobacco by the Raman spectrum according to claim 4, wherein the inorganic acid solution in the step (2) can be one or two of nitric acid and sulfuric acid, and the concentration is 1-10 mol/L.
6. The pretreatment method for detecting pesticide residues in tobacco by Raman spectroscopy according to claim 1, wherein the amount of the extracting solution added in the step (2) is 0.8-2 mL, and the amount of the nanocarbon material used is 20-60 mg based on the volume of the extracting solution.
7. The pretreatment method suitable for detecting the pesticide residue in the tobacco by the Raman spectrum according to claim 1, wherein the liquid to be detected and the nano gold/silver enhancing reagent are mixed in the step (3) according to a volume ratio of 1: 0.5-20.
8. The pretreatment method suitable for detecting the pesticide residue in the tobacco by the Raman spectrum according to claim 1, wherein any light source can be selected for the portable Raman spectrometer; the single-frequency output power is less than or equal to 500mw, the spacing is less than or equal to 1nm, the line width is less than or equal to 0.06nm, and the spectrum range is as follows: 180 and 2800cm-1And the Raman spectrum scanning time for collecting the sample is 3-50 seconds.
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| CN114113037A (en) * | 2021-11-29 | 2022-03-01 | 云南省烟草质量监督检测站 | Method for rapidly detecting dithiocarbamate pesticides in tobacco leaves |
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