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Ultra-high performance liquid chromatography-mass spectrometry detection method of triazophos in bottom mud sediment

An ultra-high-performance liquid phase and mass spectrometry detection technology, which is applied in the field of ultra-high performance liquid chromatography-mass spectrometry detection of triazophos in sediment sediments, can solve the problem of not meeting the analysis requirements of triazophos, interfering with instrument measurement results, and lack of triazophos Phosphorus detection and other problems, to achieve the effect of high sensitivity, good extraction effect, simple operation

Active Publication Date: 2017-02-22
MARINE FISHERIES RES INST OF ZHEJIANG
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Problems solved by technology

The current detection and analysis of triazophos is generally based on GC and GC-MS, but its sensitivity to triazophos is about 10ppb, which sometimes cannot meet the analysis requirements of trace triazophos in sediment sediments. The sample matrix of sediment sediments is complex. If the impurities are not removed well during the sample pretreatment process, it may directly interfere with the measurement results of the instrument, or even damage the instrument.
At present, there is no domestic method for the detection of triazophos in sediment sediments by ultra-high liquid chromatography mass spectrometry

Method used

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  • Ultra-high performance liquid chromatography-mass spectrometry detection method of triazophos in bottom mud sediment

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Embodiment

[0021] Determination of Triazophos in Bottom Mud of Loach Breeding Pond

[0022] 1. Vortex oscillation + ultrasonic solvent extraction: Weigh about 10g of wet sample into a 50ml centrifuge tube, add 10ml of pure water, then add 15ml of ethyl acetate, stopper and oscillate for 2 minutes, under the action of 40KHz ultrasonic wave for 35 Extract at ℃-45℃ for 10 minutes, then centrifuge the extracted sample for 5 minutes at 5000 rpm, separate the extract, add 15 ml of ethyl acetate to repeat the extraction once, and combine the extracts.

[0023] 2. Dispersive solid phase extraction + enrichment and purification of solid phase extraction column: add about 0.2 grams each of graphitized carbon black and N-propylethylenediamine (PSA) to the extract, vortex for 2 minutes, and centrifuge at 5000 rpm After 2 minutes, the liquid separated by centrifugation over anhydrous sodium sulfate was collected in a 100 ml chicken-shaped bottle, rotatively evaporated to dryness, and washed and disso...

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Abstract

The invention discloses an ultra-high performance liquid chromatography-mass spectrometry detection method of triazophos in bottom mud sediment. The method comprises steps as follows: (1) vortex oscillation and ultrasonic solvent extraction; (2) dispersive solid-phase extraction and solid-phase extraction column enrichment and purification: graphitized carbon black and N-propyl ethylenediamine are added to an extracting solution, vortex oscillation and centrifugation are performed, the mixture is treated with anhydrous sodium sulfate, rotary evaporation is performed until the mixture is dried, a to-be-detected liquid is obtained after n-hexane is added for washing and dissolution, the to-be-detected liquid is added to a magnesiumtrisilicate solid-phase extraction column and eluted with dichloromethane, and an eluant is collected; (3) ultra-high performance liquid chromatography-mass spectrometry detection: the eluant is taken for liquid chromatography-mass spectrometry detection, then, a standard working curve is drawn, quantification is performed with an external standard method, and the concentration of triazophos is calculated according to the peak area. The method is convenient to operate, better in reproducibility, accurate in qualitative detection and higher in recovery rate and can be used for rapidly analyzing triazophos in the bottom mud sediment.

Description

technical field [0001] The invention relates to the technical field of fishery environment monitoring, in particular to an ultra-high performance liquid chromatography mass spectrometry detection method for triazophos in sediment sediment. Background technique [0002] Triazophos is a broad-spectrum organophosphorus insecticide, acaricide, and nematocide, mainly used for the control of lepidopteran pests, harmful mites, fly larvae and insects on fruit trees, cotton, and food crops. Subterranean pests, etc., have strong contact, stomach poisoning and systemic effects. With the prohibition of most organochlorine and organophosphorus highly toxic pesticides, the demand for triazophos is increasing because it can be degraded relatively quickly in the environment, and it is difficult to be completely replaced by other pesticides in a short period of time. Shi Lili studied the degradation characteristics in three different types of soil, showing that the degradation half-lives ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72G01N2030/062
Inventor 金衍健卓丽飞孙秀梅蒋雪燕郝青严忠雍方益胡红美
Owner MARINE FISHERIES RES INST OF ZHEJIANG
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