Detection method of detecting trimethylsulfonium in tea leaves by liquid chromatograph-tandem mass spectrometer

A technology of liquid chromatography and trimethylsulfonium, applied in the detection field of trimethylsulfonium

Inactive Publication Date: 2018-08-17
镇江出入境检验检疫局检验检疫综合技术中心 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Based on the fact that mass spectrometry has not been used to detect trimethyls

Method used

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  • Detection method of detecting trimethylsulfonium in tea leaves by liquid chromatograph-tandem mass spectrometer
  • Detection method of detecting trimethylsulfonium in tea leaves by liquid chromatograph-tandem mass spectrometer
  • Detection method of detecting trimethylsulfonium in tea leaves by liquid chromatograph-tandem mass spectrometer

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[0018] The specifications of the instruments and medicines involved in the present invention are as follows:

[0019] Thermo TSQ Quantan Access liquid chromatography-tandem mass spectrometer: distributed spray ion source (ESI) and autosampler (Finnigen Surveyor); electronic balance: sensitivity 0.1mg (Mettler, Switzerland); 3K15 high-speed refrigerated centrifuge Machine (Sigma Company);

[0020] Acetonitrile is chromatographically pure (Merck, Germany); formic acid, ammonium acetate, and hydrogen peroxide are analytically pure (Shanghai Sinopharm Group); N-propyl ethylenediamine solid powder (PSA, Shanghai Anpu). The experimental water is Milli-Q high purity water. Tall beaker (30mm in diameter, 50mL). 15mL graduated centrifuge tube (Shanghai Anpu Company). Graphitized carbon black (GCB, Shenzhen Comma Company). Hydrophilic membrane (0.22um, Shanghai Anpu Company). Sample extract (0.77g ammonium acetate / 1000mL water, containing 2mL formic acid).

[0021] The standard trimethyl...

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Abstract

The invention discloses a detection method of detecting trimethylsulfonium in tea leaves by a liquid chromatograph-tandem mass spectrometer. The detection method comprises the following steps of 1) sample pretreatment; and 2) chromatogram and mass spectrum conditions of detection with liquid chromatography-tandem mass spectrometry: a mobile phase: organic phase is acetonitrile, a water phase is anammonium acetate-formic acid solution which has the concentration of 15mmol/L and contains 1.5mL of formic acid per L; gradient elution: a flow rate is 0.30mL/min, and a feeding amount is 25 microlitres; ion source: electrospray ionization (ESI) with positive ion scanning; a mass spectrum scanning manner is multiple reaction monitoring (MRM); spray voltage is 4,200V; shell gas pressure is 40arb;and collision gas (Ar/m) Torr: 1.5. By adopting the detection method, the recovery rate and the precision accord with relevant technical specifications, residues of the trimethylsulfonium in the tea leaves can be effectively detected, and the detection requirements for a residue limit of the trimethylsulfonium in the tea leaves of the European Union are met.

Description

technical field [0001] The application of the present invention relates to the detection of trimethylsulfonium in tea, especially a detection method for detecting trimethylsulfonium in tea with liquid chromatography coupled with mass spectrometry Background technique [0002] Pesticide glyphosate (glyphosate) is a broad-spectrum, post-emergence, non-selective herbicide, existing in the form of glyphosate acid or salt, common glyphosate isopropionate, glyphosate trimethyl Sulfonium salt, glyphosate potassium salt, etc. Glyphosate has good weed control effect and has been widely used all over the world. When glyphosate trimethylsulfonium salt is used as a herbicide, trimethylsulfonium (trimethylsulfonium) residues will be produced in tea leaves. For this reason, the EU has set maximum residue limits for trimethylsulfonium in tea imported into the region. Among them, the residue limit of non-organic tea is 50ug / kg; organic tea is based on the principles formulated by the Int...

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88
Inventor 周洪斌李丽王现平孙俪任丽丽
Owner 镇江出入境检验检疫局检验检疫综合技术中心
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