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Method for measuring residual quantity of imidacloprid and pymetrozin in chrysanthemum through on-line purification-LC (Liquid Chromatogram)-MS (mass spectrometry)/MS

A liquid chromatography and imidacloprid technology is applied in the field of determination of imidacloprid and pymetrozine residues in chrysanthemum, and can solve the problems of few detection methods and the like

Active Publication Date: 2016-05-04
THE INSPECTION & QUARANTINE TECH CENT ZHEJIANG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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Problems solved by technology

[0003] At present, there are few detection methods involving the determination of imidacloprid and pymetrozine residues in chrysanthemums

Method used

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  • Method for measuring residual quantity of imidacloprid and pymetrozin in chrysanthemum through on-line purification-LC (Liquid Chromatogram)-MS (mass spectrometry)/MS
  • Method for measuring residual quantity of imidacloprid and pymetrozin in chrysanthemum through on-line purification-LC (Liquid Chromatogram)-MS (mass spectrometry)/MS
  • Method for measuring residual quantity of imidacloprid and pymetrozin in chrysanthemum through on-line purification-LC (Liquid Chromatogram)-MS (mass spectrometry)/MS

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Embodiment Construction

[0055] To further illustrate the present invention, it will be specifically described in conjunction with the following embodiments:

[0056] 1. Reagents and materials

[0057] 1.1 Ultra-pure water;

[0058] 1.2 Acetonitrile: chromatographically pure;

[0059] 1.3 Formic acid: chromatographically pure;

[0060] 1.40.1% formic acid solution: accurately pipette 1.0 mL of formic acid and dilute to 1000 mL with water.

[0061] 1.5 Standard products: See Table 4 for information.

[0062] Table 4 Standard product information

[0063] Compound

English name

CAS number

Imidacloprid

Imidacloprid

138261-41-3

Pymetrozine

Pymetrozin

123312-89-0

[0064] 2. Instruments and equipment

[0065] 2.1 Online purification-liquid chromatography-mass spectrometer / mass spectrometer, equipped with electrospray ion source;

[0066] 2.2 Homogenizer;

[0067] 2.3 Centrifuge.

[0068] 3. Measurement steps

[0069] 3.1 Sample preparation

[0070] Weigh 1.00g of sample, put it in a 50mL plastic centrifuge tube, ...

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Abstract

The invention relates to a method for measuring the residual quantity of imidacloprid and pymetrozin in chrysanthemum, in particular to a method for quantitatively detecting imidacloprid and pymetrozin in chrysanthemum through on-line purification-LC (Liquid Chromatogram)-MS (mass spectrometry) / MS. The method comprises the following steps: weighing a sample of 1.00g, putting the sample into a plastic centrifuge tube of 50ml, adding water of about 20ml for immersing the sample for 30 minutes, homogenizing, adding acetonitrile of 20ml and sodium chloride of about 4g, whirling for 3 minutes, centrifuging, filtering an upper solution of about 1ml through a membrane, purifying on line, and measuring through an LC-MS / MS instrument. The method is used for measuring the residual quantity of imidacloprid and pymetrozin in chrysanthemum through on-line purification-LC-MS / MS, is simple, convenient, quick, accurate and reliable, and can ensure that the limit of detection, the recovery rate and the precision all meet requirements.

Description

Technical field [0001] The invention relates to a method for determining imidacloprid and pymetrozine residues in chrysanthemums, in particular to a method for quantitatively detecting imidacloprid and pymetrozine in chrysanthemums by online purification-liquid chromatography-mass spectrometry / mass spectrometry. Background technique [0002] Chrysanthemum is a commonly used medicinal material, which is included in the Chinese Pharmacopoeia. It has the functions of clearing the liver and promoting gallbladder, invigorating the stomach and reducing food, diuresis and swelling; it is also often used as a drink. Imidacloprid and pymetrozine are pyridine insecticides with broad-spectrum, high-efficiency, and low-toxicity characteristics. They can effectively prevent and control aphids during the flowering period of chrysanthemums. They are effective pesticides recommended to chrysanthemum farmers for use by relevant departments. This kind of pesticide will inevitably produce certain r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/28
CPCG01N30/02G01N30/28
Inventor 黄超群谢文蒋沁婷李慧思楼成杰吴娟黄雷芳
Owner THE INSPECTION & QUARANTINE TECH CENT ZHEJIANG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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