Method for simultaneously detecting trifloxystrobin and metabolite trifloxystrobin acid residual in rice by LC-MS/MS (Liquid Chromatography-Tandem Mass Spectrometry)

A technology for trifloxystrobin and metabolites, applied in the field of simultaneous detection of food safety, can solve the problems of complex matrix, inability to accurately quantify target compounds, inability to achieve effective separation of target compounds, etc. Effect

Inactive Publication Date: 2017-03-29
PLANT PROTECTION & QUALITY & SAFETY OF AGRI PRODS INST ANHUI ACAD OF AGRI SCI
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Problems solved by technology

However, the matrix of rice is complex, especially when the purification of the sample matrix is ​​not complete, the target compound cannot be effectively separated on the chromatographic column,

Method used

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  • Method for simultaneously detecting trifloxystrobin and metabolite trifloxystrobin acid residual in rice by LC-MS/MS (Liquid Chromatography-Tandem Mass Spectrometry)
  • Method for simultaneously detecting trifloxystrobin and metabolite trifloxystrobin acid residual in rice by LC-MS/MS (Liquid Chromatography-Tandem Mass Spectrometry)
  • Method for simultaneously detecting trifloxystrobin and metabolite trifloxystrobin acid residual in rice by LC-MS/MS (Liquid Chromatography-Tandem Mass Spectrometry)

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[0028] Example 1

[0029] (1) Weigh 10.0 g of crushed rice samples that can pass through a 20-mesh sieve, and first use 40 mL of acetonitrile-water solution containing 0.01% (volume ratio) of formic acid and 75% (volume ratio) to extract the sample by shaking for 30 minutes;

[0030] (2) adding 5.0g sodium chloride in the sample extract to carry out salting out, shaking for 5min, and centrifuging;

[0031] (3) Take 1.5mL of the supernatant after centrifugation into a centrifuge tube, add 50mg C 18 and 150 mg of magnesium sulfate, vortexed for 2 min, centrifuged at 5000 r / min for 5 min, took the supernatant and passed through a 0.22 μm microporous filter membrane, pipet 600 μL into the injection bottle, added 400 μL of acetonitrile, and mixed evenly to obtain the sample analysis solution. solution, to be tested;

[0032] (4) Utilizing ultra-high performance liquid chromatography tandem mass spectrometry method to simultaneously detect tristrobin and the metabolite tristrobin ...

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Abstract

The invention discloses a method for simultaneously detecting trifloxystrobin and metabolite trifloxystrobin acid residual in rice by LC-MS/MS (Liquid Chromatography-Tandem Mass Spectrometry). The method comprises the following steps: extracting a to-be-detected rice sample; salting out a sample extracting solution; adding sodium chloride in the sample extracting solution for salting out, oscillating and centrifuging; purifying the sample subjected to salting out and diluting with acetonitrile; simultaneously detecting the trifloxystrobin and the metabolite o trifloxystrobin acid in the sample analysis solution by using a UPLC-MS/MS (Ultra High Performance LC-MS/MS) method. According to the method disclosed by the invention, a rice test sample is extracted with water and an acetonitrile mixed solution containing formic acid, then is purified by a matrix solid-phase extraction technology, and is subsequently and simultaneously detected under a multi-reaction monitoring (MRM) mode by using the UPLC-MS/MS, so that the simultaneous detection efficiency is improved, and the simultaneous detection cost is reduced; the method has the advantages of low detection limit, high sensitivity, good repeatability and high addition standard recovery rate.

Description

technical field [0001] The present invention relates to a method for simultaneous detection of trifloxystrobin and metabolite trifloxacin residues in rice by LC-MS / MS, in particular to the simultaneous detection of oxime in rice by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS / MS) The method for strobilurin and its metabolite oxalic acid belongs to the field of simultaneous detection of food safety. Background technique [0002] Trifloxystrobin broad-spectrum fungicides are a new class of fluorine-containing fungicides successfully developed from natural products Strobilurins as fungicide lead compounds. It has the characteristics of high efficiency, broad spectrum, protection, treatment, eradication, penetration, systemic activity, resistance to rain erosion, and long-lasting effect. It is effective for strains resistant to 1,4-demethylase inhibitors, benzamides, dicarboxylamines and benzimidazoles, and has no cross-resistance with existin...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/34
CPCG01N30/02G01N30/06G01N30/34G01N2030/062
Inventor 段劲生孙明娜高同春董旭王梅肖青青褚玥
Owner PLANT PROTECTION & QUALITY & SAFETY OF AGRI PRODS INST ANHUI ACAD OF AGRI SCI
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