High performance liquid chromatography-time-of-flight mass spectrometry hyphenated method capable of simultaneously and rapidly screening and identifying alkaloid in water sample

A technology of high-performance liquid chromatography and time-of-flight mass spectrometry, which is applied in the field of analytical chemistry and can solve problems such as alkaloid composition and concentration detection

Inactive Publication Date: 2013-10-23
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The prior art cannot address the problem of detecting the composition and concentration of alkaloids in environmental media. The present invention provides a high performance liquid chromatography-time-of-flight mass spectrometry method for simultaneous and rapid screening and identification of alkaloids in water samples, which can be used in In a separate analysis and determination, the primary and secondary mass spectra of unknown compounds in the water sample are scanned and screened in rapid succession, and the primary and secondary mass spectrograms of different substances are extracted and analyzed and compared with the existing Some substance libraries are compared, and then the probability of the existence of a certain substance is judged by the scoring value given by the software. The qualitative evaluation is comprehensive and comprehensive, which can realize the function of comprehensive screening of non-target alkaloid pollutants that cannot be achieved by traditional instruments.

Method used

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  • High performance liquid chromatography-time-of-flight mass spectrometry hyphenated method capable of simultaneously and rapidly screening and identifying alkaloid in water sample
  • High performance liquid chromatography-time-of-flight mass spectrometry hyphenated method capable of simultaneously and rapidly screening and identifying alkaloid in water sample
  • High performance liquid chromatography-time-of-flight mass spectrometry hyphenated method capable of simultaneously and rapidly screening and identifying alkaloid in water sample

Examples

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Embodiment 1

[0049] A high-performance liquid chromatography-time-of-flight mass spectrometry method for simultaneous rapid screening and identification of alkaloids in water samples, the steps of which are:

[0050] (A) Membrane filtration: Take 1L of the primary effluent collected from the sewage treatment plant near the farm and pass through two layers of filter membranes through a glass vacuum filter; the two layers of filter membranes used are 1um glass fiber filter membrane and 0.45um nylon filter membrane.

[0051] (B) Solid-phase extraction: use the solid-phase extraction column to enrich the alkaloids contained in the water sample; the solid-phase extraction column is the C18 column of Oasis HLB, and use the mass ratio of A 1:1 mixed solvent of dichloromethane and methanol and deionized water were activated; the flow rate was kept at 5mL / min during the enrichment process, and the column was kept wet throughout the process.

[0052] (C) Solvent elution: Use an organic solvent to elu...

Embodiment 2

[0071] The secondary effluent of the sewage treatment plant was treated as in Example 1, and similar instrument measurements and data analysis were also carried out to obtain the same three alkaloid drugs codeine (codeine) and pavaverine as in the primary effluent water sample (papaverine).

[0072] The above two examples can show that there are indeed alkaloid drugs in the wastewater of the sewage treatment plant, and the existing treatment process of the sewage treatment plant cannot remove such drugs.

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Abstract

The invention discloses a high performance liquid chromatography-time-of-flight mass spectrometry hyphenated method capable of simultaneously and rapidly screening and identifying alkaloid in a water sample, belonging to the field of analytical chemistry. The method comprises the steps of (A) filtering a filter membrane; (B) extracting a solid phase columella; (C) eluting a solvent; (D) concentrating and metering the volume; and (E) detecting on a machine, wherein the sample is screened and identified by a high performance liquid chromatography--time-of-flight mass spectrometry. The high performance liquid chromatography-time-of-flight mass spectrometry is adopted for testing and is cooperated with the analytical method of a peak view comprehensive assessment grading software to screen and survey the water sample in large scale, the water sample is scanned under a first mass spectrum mode and a second mass spectrum mode, the resolution ratio is high, the accuracy is high, the scanning and a compound substance library are matched through a second mass spectrum spectrogram peak shape, the quantitative advantage is obvious, the result of purity score is displayed concisely and intuitively, and the result is more accurate and reliable.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, in particular, it relates to a method for simultaneous rapid screening and identification of alkaloid compounds in sewage treatment plant wastewater, more specifically, a method for simultaneous rapid screening and identification of alkaloids in water samples High performance liquid chromatography-time-of-flight mass spectrometry method. Background technique [0002] With the increasing use of drugs and the complexity and diversification of their types caused by medical progress, the probability of these daily sewage containing compounds such as drugs being discharged into the environmental medium after being metabolized by the human body is greatly increased. However, the potential risk of the active compounds in these drugs to the environment is still unclear, and further exploration and research are needed. [0003] Alkaloids are the earliest studied biologically active natural organic com...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 韦斯胡梦阳于红霞于南洋李俊李梅映
Owner NANJING UNIV
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