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A method for detecting the residual amount of dichlorcap in tobacco

A detection method, the technology of dinocap, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of poor selectivity, precision and reproducibility, cumbersome and time-consuming processing and extraction steps, long hydrolysis time, etc., and achieve sensitivity and high accuracy, simple and fast purification steps, and simple detection methods

Active Publication Date: 2021-11-02
YUNNAN ACAD OF TOBACCO AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The pretreatment and extraction steps of liquid chromatography or liquid chromatography-mass spectrometry are cumbersome and time-consuming. It is necessary to completely hydrolyze all six isomers of dinocap into phenols. The hydrolysis time is long, and because dinocap cannot be purchased The standard substance of general hydrolyzed phenol is difficult to quantify accurately; the selectivity, precision and reproducibility are poor when analyzed by gas chromatography-ECD method

Method used

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  • A method for detecting the residual amount of dichlorcap in tobacco
  • A method for detecting the residual amount of dichlorcap in tobacco

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Embodiment 1

[0035]1. Instruments and reagents: Bruker 450GC-300MS gas chromatography-tandem mass spectrometer (Bruker, USA), Millipore ultrapure water machine (Millipore Simplicity, USA), Eppendorf 5804 high-speed centrifuge (Eppendorf, Germany), Talboys digital display multi Tubular vortex mixer (Shanghai Anpu Scientific Instrument Co., Ltd.). Methanol, acetonitrile, formic acid, 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, analytically pure. Dinocap standard substance (purity 98%, provided by Dr. Germany).

[0036] 2. Detection method of dichlorcap residues in tobacco:

[0037] 1) Preparation of standard solution: Accurately weigh dinocap standard product (accurate to 0.1 mg), dissolve in methanol and dilute to 100mL brown volumetric flask, make a single standard stock solution of 1 mg / L, st...

Embodiment 2

[0052] A method for detecting residues of dichlorcap in tobacco, comprising the following steps:

[0053] 1) Preparation of standard solution: Accurately weigh 0.1 g of dinocap standard product to the nearest 0.1 mg, dissolve in methanol and dilute to a 100 mL brown volumetric flask, prepare a 1 mg / mL standard stock solution, and store in a -15°C refrigerator Store in the dark, dilute the standard stock solution into a series of standard working solutions for making a standard curve;

[0054] The method for making the standard curve is specifically to use methanol to prepare the dinocap standard stock solution into 0.01, 0.02, 0.05, 0.1, 0.2 and 0.5 mg / L serial mass concentrations of dinocap standard working solutions, and compare the peak area with the dinocap standard working solution. Linear regression was carried out at each concentration to obtain a standard curve. The standard curve was good linear in the range of 0.01-0.5 mg / L when the dinocap mass concentration was 0.0...

Embodiment 3

[0063] A method for detecting residues of dichlorcap in tobacco, comprising the following steps:

[0064] 1) Preparation of standard solution: Accurately weigh 0.1 g of dinocap standard product, accurate to 0.1 mg, dissolve in methanol and dilute to 100mL brown volumetric flask, prepare 1mg / mL standard stock solution, store in -25℃ refrigerator Store in the dark, dilute the standard stock solution into a series of standard working solutions for making a standard curve;

[0065] The method for making the standard curve is specifically to use methanol to prepare the dinocap standard stock solution into 0.01, 0.02, 0.05, 0.1, 0.2 and 0.5 mg / L serial mass concentrations of dinocap standard working solutions, and compare the peak area with the dinocap standard working solution. Linear regression was carried out at each concentration to obtain a standard curve. The standard curve was good linear in the range of 0.01-0.5 mg / L when the dinocap mass concentration was 0.01-0.5 mg / L, and...

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Abstract

The invention discloses a method for detecting the residual amount of dinocap in tobacco. Tobacco samples were extracted by the improved QuEChERS technology extraction method, C18 dispersive adsorbent, detected by gas chromatography negative chemical source mass spectrometry, and quantified by external standard method. The results showed that dinocap had a good linear relationship in the range of 0.01‑0.5 mg / L , the correlation coefficient (r 2 ) was greater than 0.99, the detection limit was 0.02 mg / kg, the recovery rate of dinocap in tobacco was 95.83%-102.34%, and the relative standard deviation was 3.75%-5.30%. The detection method sample pretreatment is simple and fast, and the sensitivity, accuracy and precision all meet the requirements of pesticide residue detection, and it is suitable for the detection of dinocap residues in tobacco.

Description

technical field [0001] The invention belongs to the technical field of pesticide residue detection technology, and in particular relates to a detection method for dichlorcap residues in tobacco. Background technique [0002] Dinocap (CAS: 39300-45-3) is a mixture of six different dinitrocrotonate isomers. It is a contact fungicide and is mainly used to control crops and fruits and vegetables. powdery mildew, and additionally acts as a non-systemic acaricide. Dificap is highly toxic, teratogenic and carcinogenic. Improper application will cause residues in crops and seriously affect the quality and safety of tobacco leaves. Therefore, all countries have formulated very strict MRL values. CORESTA Guidance Residue Limits (GRL ) stipulates that dinocap in tobacco is 0.6 mg / kg, and China National Tobacco Corporation stipulates that the maximum residue limit (MRL) of dinocap in tobacco is 0.1 mg / kg, so the detection of its residue is very important. [0003] Due to the thermal a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/72
CPCG01N30/02G01N30/06G01N30/14G01N30/72
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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