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Method for determining chloramphenicol in freshwater pond sediment by applying liquid chromatograph/mass spectrometer

A technology of pond sediment and combined instrument, applied in the fields of ecological environment safety and analytical chemistry, can solve the problems of unfavorable accurate qualitative and quantitative analysis, cumbersome operation steps, large analysis interference, etc., so as to optimize the pretreatment process and simplify the operation steps. , the effect of high sensitivity

Inactive Publication Date: 2015-03-11
农业部渔业环境及水产品质量监督检验测试中心(天津)
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AI Technical Summary

Problems solved by technology

[0006] Due to the complex composition and many impurities in freshwater aquaculture pond sediment, the analysis is greatly disturbed. The detection method of gas-liquid chromatography needs to be derivatized, and the purification requirements for samples are high. The entire operation steps are cumbersome and time-consuming. The detection of chromatographic instruments is easy to form similar peak interference and poor thermal stability, which is not conducive to accurate qualitative and quantitative analysis. Therefore, it is necessary to develop a detection method with low interference, high stability and accurate data.

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  • Method for determining chloramphenicol in freshwater pond sediment by applying liquid chromatograph/mass spectrometer
  • Method for determining chloramphenicol in freshwater pond sediment by applying liquid chromatograph/mass spectrometer
  • Method for determining chloramphenicol in freshwater pond sediment by applying liquid chromatograph/mass spectrometer

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Experimental program
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Effect test

Embodiment 1

[0066] Embodiment 1 The selection of parent ion

[0067] The hydroxyl functional group in chloramphenicol can be negatively charged, and the (ESI-) ionization mode can provide more fragment information than the (ESI+) positive ion mode, and the sensitivity is greatly improved, such as figure 1 As shown, in this method, the 0.5 mg / L chloramphenicol standard solution and the chloramphenicol-D5 internal standard solution are continuously injected at a speed of 10 μl / min by a flow syringe pump to perform a full scan of the precursor ion in the negative ion mode to determine the chlorine The molecular ions of chloramphenicol and chloramphenicol-D5 are m / z 321.1 and 326.1, respectively.

[0068] Then use their respective parent ions to perform secondary mass spectrometry scanning analysis in the way of product ion scanning to find out two characteristic fragment ions with relatively strong selection abundance, monitor ion pairs with parent ions and product ions, and monitor with mu...

Embodiment 2

[0069] Example 2 Sample pretreatment conditions

[0070] Sample pretreatment

[0071] The invention is based on the bottom mud samples of freshwater ponds. The substrate in the bottom mud of freshwater ponds is very complicated, the interference is large, and the pretreatment is very complicated.

[0072] The bottom sediment samples of the breeding ponds were collected, and the surface sediments were collected with a mud picker, and stored in a jar at -18°C.

[0073] This is because the chloramphenicol used in the fish farming process is enriched in the surface sediment through water and fish metabolism.

[0074] Sample extraction: Weigh 5.00g (±0.01g) of the sample and place it in a 50ml centrifuge tube, add 2ml of water to moisten it for better extraction later. Accurately add 500μl 10.0ng / ml chloramphenicol internal standard solution, add 5ml of acetonitrile, 5ml of 4% sodium chloride solution to increase the extraction effect, vortex for 2min, ultrasonically extract for ...

Embodiment 3

[0086] Example 3 Determination of detection conditions of liquid-mass-mass spectrometer

[0087] According to the relevant provisions of CAC and EU Resolution No. 657 / 2002 / EEC, two pairs of ions can be selected for MRM monitoring to meet the detection requirements. At the same time, the selection of product ions mainly considers the parent ion and product ion according to the mass spectrum and structure of each compound. Characteristic selection, and the matrix interference is less in the actual sample analysis. After determining the molecular ions of various substances according to the above principles, the molecular ions of various compounds are respectively used as parent ions, and the product ions are selected for a full scan. , The two pairs of product ions with less interference are qualitative ions, and the strongest pair is quantitative ions. Finally, various mass spectrometry parameters are optimized in the positive ion mode of multiple reaction monitoring (MRM).

[0...

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Abstract

The invention relates to a method for determining chloramphenicol in freshwater pond sediment by applying a liquid chromatograph / mass spectrometer. The method comprises the following steps of firstly, collecting a sediment sample of an aquaculture pond; secondly, extracting the sample; thirdly, purifying with n-hexane; fourthly, extracting water saturated ethyl acetate solution; fifthly, blowing extracting solution to be dry with nitrogen gas, and dissolving the dry extracting solution with acetonitrile-water (5+95) to obtain standby solution; sixthly, performing solid phase extraction column for eluting; seventhly, extracting the water saturated ethyl acetate solution, and blowing dry with the nitrogen gas; eightly, dissolving methanol water (50+50), whirling, filtering by a microfiltration membrane of 0.22[mu]m and determining by using the liquid chromatograph / mass spectrometer. According to the method disclosed by the invention, by pretreatment for the freshwater pond sediment, a matrix disturbing substance is removed, the sensitivity is improved, and the pretreatment process is optimized; in addition, the sample is prevented from being derivaed, so that the operation step is simplified; a reliable detection means can be provided for checking a pollution source and evaluating the influence of the ecological environment on healthy breeding.

Description

technical field [0001] The invention belongs to the technical fields of analytical chemistry and ecological environment safety, in particular to a method for measuring chloramphenicol in bottom mud of freshwater ponds by using a liquid-mass spectrometer. Background technique [0002] Chloramphenicol (CAP) is a broad-spectrum antibiotic that is effective against aerobic and anaerobic bacteria, as well as chlamydia, mycoplasma, and rickettsia. Due to its low price and remarkable effect, it is often used as medicine for the treatment and prevention of diseases in livestock, poultry and aquatic products. However, chloramphenicol has serious toxic and side effects, which can inhibit the hematopoietic function of human bone marrow and easily cause aplastic anemia, agranulocytosis and gray baby syndrome. Therefore, in order to ensure the safety of animal-derived food and ensure that the drug does not cause harm to humans, countries around the world have made strict regulations on ...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 张素青陈永平李春青叶红梅高丽娜李连庆时文博王秀芹王德兴王宝峰马丹王娟娟易伟李兆千张玲
Owner 农业部渔业环境及水产品质量监督检验测试中心(天津)
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