Method for Determination of Chloramphenicol in Freshwater Pond Sediment Using LC-MS
A pond sediment and combined instrument technology, which is applied in the field of ecological environment safety and analytical chemistry, can solve the problems of unfavorable accurate qualitative and quantitative analysis, cumbersome operation steps, and large analysis interference, so as to optimize the pretreatment process and simplify the operation steps , the effect of improving the sensitivity
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Embodiment 1
[0066] The selection of embodiment 1 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. This is because the chloramphenicol used in the fish farming process is enriched in the surface sediment through water and fish metabolism.
[0073] 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 20min, an...
Embodiment 3
[0085] Embodiment 3 Determination of detection conditions of liquid-mass-mass spectrometry instrument
[0086] 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 ...
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