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Method for detecting meptyldinocap residue amount in tobaccos

A technology of nifedimetholone and a detection method, applied in the field of detection of nifedimethoxin residues in tobacco, can solve the problems of poor selectivity, precision and reproducibility, thermal and chemical instability, and complicated operation steps. Time-consuming and other issues, to achieve the effect of high sensitivity and accuracy, timely detection, and short analysis time

Active Publication Date: 2017-12-01
YUNNAN ACAD OF TOBACCO AGRI SCI
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Problems solved by technology

[0003] At present, the detection methods reported abroad include high performance liquid chromatography, gas chromatography-ECD method, gas chromatography-mass spectrometry, and liquid chromatography-mass spectrometry. Because the drug has thermal and chemical instability, it is easy to hydrolyze Or photolysis into corresponding phenols, so selectivity, precision and reproducibility are poor when analyzed by gas chromatography (GC) or gas chromatography-mass spectrometry (GC-MS), and LC method has poor sensitivity and selectivity, resistance The disadvantage of weak matrix interference ability, LC-MS / MS has the advantages of high sensitivity and selectivity
The LC method or LC-MS / MS method is mainly used to calculate the residual amount of the parent body by analyzing the residual amount of the hydrolyzed product phenol corresponding to metystrobin. The method currently reported mainly uses organic solvent extraction, after liquid-liquid distribution, adding Sodium hydroxide solution is hydrolyzed into corresponding phenols. These methods are cumbersome and time-consuming, and easily cause the loss of target pesticides

Method used

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  • Method for detecting meptyldinocap residue amount in tobaccos
  • Method for detecting meptyldinocap residue amount in tobaccos
  • Method for detecting meptyldinocap residue amount in tobaccos

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Experimental program
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Effect test

Embodiment 1

[0031]1. Instruments and reagents: ultra-high performance liquid chromatography (Waters, USA), AB Sciex QTRAP 5500 mass spectrometer (AB Sciex, USA), Millipore Simplicity personal ultrapure water machine (Millipore, USA), Eppendorf 5804 high-speed centrifuge (Germany Eppendorf), Talboys digital multi-tubular vortex mixer (Shanghai Anpu Scientific Instrument Company). Methanol, acetonitrile, HPLC grade, American Fisher Company. Anhydrous magnesium sulfate, analytically pure. It should be burned at 650°C for 4 hours before use, and stored in a desiccator for later use. Sodium chloride, sodium citrate, disodium hydrogen citrate, sodium hydroxide, ammonia water, analytically pure. 2,4-DNOP and 2,4-DNOPC standard products (purities were 98.5% and 93%, respectively, provided by Dr Company in Germany).

[0032] 2. Detection method for the residual amount of metystrobin in tobacco:

[0033] 1) Preparation of standard solution: Accurately weigh 2,4-DNOPC and 2,4-DNOP standard (accu...

Embodiment 2

[0056] A kind of detection method of mechlorstrobin residual amount in tobacco, comprises the following steps:

[0057] 1) Preparation of standard solution: Accurately weigh 2,4-DNOP standard product, accurate to 0.1 mg, dissolve in methanol and dilute to 100mL brown volumetric flask, make a single standard stock solution of 1mg / L, store in -20℃ refrigerator Store in dark place, used for making standard curve and quantitative detection;

[0058] The preparation of the standard curve is specifically to use the tobacco blank matrix extract to prepare 2,4-DNOP matrix matching standard working solutions with a series of mass concentrations of 0.001, 0.002, 0.005, 0.01, 0.02, 0.05, 0.1, 0.2 and 0.5 mg / L , each concentration is carried out linear regression with peak area, obtains standard curve, and described standard curve is good linearity in the range of 0.001-0.5 mg / L in 2,4-DNOP mass concentration, correlation coefficient r 2 Greater than 0.999;

[0059] Prepare 2,4-DNOPC st...

Embodiment 3

[0065] A kind of detection method of mechlorstrobin residual amount in tobacco, comprises the following steps:

[0066] 1) Preparation of standard solution: Accurately weigh 2,4-DNOP standard product, accurate to 0.1 mg, dissolve in methanol and dilute to 100mL brown volumetric flask, make a single standard stock solution of 1mg / L, store in -20℃ refrigerator Store in dark place, used for making standard curve and quantitative detection;

[0067] The preparation of the standard curve is specifically to use the tobacco blank matrix extract to prepare 2,4-DNOP matrix matching standard working solutions with a series of mass concentrations of 0.001, 0.002, 0.005, 0.01, 0.02, 0.05, 0.1, 0.2 and 0.5 mg / L , each concentration is carried out linear regression with peak area, obtains standard curve, and described standard curve is good linearity in the range of 0.001-0.5 mg / L in 2,4-DNOP mass concentration, correlation coefficient r 2 Greater than 0.999;

[0068] Step (1) also includ...

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Abstract

The invention discloses a method for detecting meptyldinocap residue amount in tobaccos. The meptyldinocap residue amount in the tobaccos is detected by detecting a corresponding hydrolysis product (2,4-dinitro-6-(1-methylheptyl) phenol, 2,4-DNOP) of meptyldinocap (2,4-dinitro-6-(1-methylheptyl) phenyl crotonate, 2,4-DNOPC). Tobacco samples are extracted by an improved method, sample introduction analysis is performed after heating ultrasonic hydrolysis under an alkaline condition, detection is performed by an ultra-high performance liquid chromatography-tandem mass spectrum negative ion multi-reaction monitoring mode, quantification is performed by an external standard method, results show that the linear relationship of the meptyldinocap is good within the range of 0.001-0.5mg / L, a correlation coefficient (r2) is larger than 0.999, detection limit is 3 micrograms / kg, the recovery rate of the 2,4-DNOPC is 92.37%-100.52%, and relative standard deviation (RSD) is 2.43%-3.30%. According to the method, sample pretreatment is simple and rapid, analysis time is short, sensitivity, accuracy and precision meet pesticide residue detection requirements, and the method is applicable to detection of the meptyldinocap residue amount in the tobaccos.

Description

technical field [0001] The invention belongs to the technical field of pesticide residue detection technology, and in particular relates to a method for detecting the residual amount of medistrobin in tobacco. Background technique [0002] Meptyldinocap, 2,4-dinitro-6-(1-methylheptyl)phenyl crotonate (2,4-dinitro-6-(1-methylheptyl)phenyl crotonate, 2,4 -DNOPC), CAS: 131-72-6) is a new type of fungicide for powdery mildew, which is mainly used for the prevention and control of powdery mildew of crops and fruit trees. Memethystrobin is a single isomer isolated from six isomers of the fungicide (mite) dinocap (dinocap, CAS: 39300-45-3), which was developed by Dow AgroSciences, Inc. It has been registered for use in Europe, the United States, China and other countries. Compared with dinocap, which has a long service life, the toxicity of metystrobin has improved, but it is still a highly toxic pesticide. The maximum residue limit (MRL, the sum of 2,4-DNOPC and 2,4-DNOP), such ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/06G01N30/14
CPCG01N30/02G01N30/06G01N30/14G01N30/72G01N2030/146
Inventor 师君丽孔光辉李勇逄涛吴玉萍陈萍
Owner YUNNAN ACAD OF TOBACCO AGRI SCI
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