Method for detecting various pesticide residues in tobacco by utilizing multiwalled carbon nanotube
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A technology for multi-walled carbon nanotubes and pesticide residues, which is used in measuring devices, instruments, scientific instruments, etc.
Inactive Publication Date: 2015-07-15
ZHENGZHOU TOBACCO RES INST OF CNTC +1
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At present, in the analysis of pesticide residues, carbon nanotubes are mainly used as solid-phase extraction column fillers to enrich pesticide residues in water, and multi-walled carbon nanotubes have not been used as adsorbents for reverse solid-phase dispersion methods for various pesticide residues in tobacco. detection report
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[0024] Liquid chromatography conditions: Chromatographic column: Atlantis dC18 column (150 mm × 2.1 mm × 3 μm); column temperature: 25 ℃; injection volume: 10 μL; mobile phase: A water (containing 0.1% formic acid), B acetonitrile, Gradient elution conditions: initial acetonitrile was 10%, changed to 50% after 1 min, kept for 4 min, changed to 60% after 11 min, changed to 80% after 9 min, changed to 95% after 5 min, kept for 10 min , change to 10% after 0.01 min, and keep for 10 min; flow rate: 0.2 mL / min;.
[0025] Mass Spectrometry Conditions: Electrospray Ionization Source (ESI); Positive Ion Mode; Collision Gas: 41 kPa (6 psi); Curtain Gas: 138 kPa (20 psi); Nebulizer Gas: 345 kPa (50 psi); Auxiliary Heating Gas: 345 kPa (50 psi); electrospray voltage: 5500 V; ion source temperature: 500 ℃; scan mode: multiple reaction monitoring MRM mode; dwell time: 20 ms. The mass spectrometry parameters are shown in Table 2.
[0026]
[0027]
[0028] The concentrations of matr...
example 2
[0033] Gas chromatography conditions: chromatographic column: TR-PesticideⅡ (30 m×0.25 mm×0.25 μm); inlet temperature: 250 ℃; injection volume: 1 μL; injection method: splitless injection; carrier gas: helium , constant flow mode, flow rate 1.2 mL / min; temperature program: initial temperature 90 ℃, maintain 5 min, increase to 180 ℃ at 25 ℃ / min, maintain 15 min, increase to 280 ℃ at 5 ℃ / min, maintain 6.5 min , rising to 300 ℃ at 40 ℃ / min and keeping for 5 min;
[0034] Mass spectrometry conditions: ionization mode: electron bombardment ionization, ionization energy 70 eV; ion source temperature: 250 ℃, transfer line temperature: 280 ℃; Q2 collision gas: argon, 1.2 mTorr; scanning method: multiple reaction monitoring MRM mode. The mass spectrometry parameters are shown in Table 4.
[0035]
[0036] The concentrations of matrix-matched standard working solutions were 0.002, 0.005, 0.01, 0.02, 0.05, 0.1 and 0.2 μg / mL, respectively. These standard solutions were detected by ...
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Abstract
The invention discloses a method for detecting various pesticide residues in tobacco by utilizing a multiwalled carbon nanotube. The method is characterized in that an organic solvent is used for extraction; the multiwalled carbon nanotube is used as a reverse solid phase dispersion adsorbent; the tobacco samples are purified through vortex and centrifugation; a high performance liquid chromatography-tandem mass spectrum coupled technology and a gas chromatography-tandem mass spectrum coupled technology are combined to realize the synchronous detection of various pesticide residues in the tobacco. According to the method, the multiwalled carbon nanotube is used as the reverse solid phase dispersion adsorbent, so that the purification effect, the influence on the adsorption of the target analyte due to the frequently-used polar adsorbents is eliminated while the matrix effects are reduced, and a cleaner solution is provided to decrease the maintenance of the instrument in the using process; the multiwalled carbon nanotube is low in preparation cost and less in dosage and has the effect of greatly reducing the experimental cost; the method provided by the invention has the advantages of being correct in measurement, high in sensitivity and good in repeatability, and has the effect of satisfying the requirement for rapidly analyzing and detecting the large batch samples.
Description
technical field [0001] The invention belongs to the technical field of pesticide residue detection in tobacco, and in particular relates to a method for detecting multiple pesticide residues in tobacco by using multi-walled carbon nanotubes. Background technique [0002] Tobacco is an important economic crop in my country, and pests and diseases are important factors affecting the yield and quality of tobacco in my country. For the control of plant diseases and insect pests, chemical control is one of the main measures adopted in production. The use of pesticides has played a positive role in increasing the yield of tobacco leaves and ensuring the quality of tobacco leaves, but it has also caused an increase in pesticide residues in tobacco leaves, which has aroused strong concern from the tobacco industry and the whole society. In order to achieve accurate and rapid analysis and detection of large batches of samples, people are paying more and more attention to high-throug...
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