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An online microwave-assisted chiral derivatization-liquid mass spectrometry analysis system and method

A microwave-assisted, liquid-mass spectrometry technology, applied to the analysis of materials, material separation, instruments, etc., can solve the problems of cumbersome operation, less use of derivatization reagents, and long time, and achieve the goal of overcoming long time, short time consumption, Simple operation effect

Inactive Publication Date: 2018-09-14
SOUTH CHINA UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to overcome the disadvantages of long time required for sample pretreatment and cumbersome operation of the chiral derivatization reagent method in the prior art, the purpose of the present invention is to provide an online microwave-assisted chiral derivatization-LC-MS analysis system, which can Pattern-derived chiral compounds, short reaction time, less use of derivatization reagents, automatic control, high sensitivity, online sample pretreatment, separation and detection, reducing human error and improving precision and accuracy

Method used

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  • An online microwave-assisted chiral derivatization-liquid mass spectrometry analysis system and method
  • An online microwave-assisted chiral derivatization-liquid mass spectrometry analysis system and method
  • An online microwave-assisted chiral derivatization-liquid mass spectrometry analysis system and method

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Embodiment 1

[0037] Such as figure 1 As shown, the online microwave-assisted chiral derivatization-liquid chromatography-mass spectrometry analysis system of this embodiment includes an online microwave-assisted chiral derivatization device and a liquid chromatography / mass spectrometry device.

[0038] The on-line microwave-assisted chiral derivatization device includes a first chromatographic pump 1 for pushing acetonitrile, an autosampler 4 for introducing samples, a two-way mixer 5 and a microwave synthesizer 7 connected sequentially through pipelines; The acetonitrile pushed by a chromatographic pump 1 flows through the reaction tube 6 in the autosampler 4, the two-way mixer 5, and the microwave synthesizer 7 in sequence;

[0039] The liquid chromatography / mass spectrometry device includes a second chromatographic pump 2 for pushing the first mobile phase, a third chromatographic pump 3 for pushing the second mobile phase, a six-way switching valve 9 for flow path switching, Three-way...

Embodiment 2

[0050] The online microwave-assisted chiral derivatization-UPLC-MS / MS system of this embodiment is the same as that of Embodiment 1.

[0051] Using the online microwave-assisted chiral derivatization-UPLC-MS / MS system of this example to analyze the product of the microwave derivatization reaction of Bambuterol in human plasma, the process is as follows:

[0052] 1. Extraction of bambuterol in plasma by liquid-liquid extraction: pipette 90 μL of human plasma sample (containing 30.00 μg / mL neostigmine methylsulfate) into a labeled EP tube, add 10 μL of bambuterol solution , and then add 100 μL of 1M sodium carbonate aqueous solution, and vortex for 2 min. Add 1 mL of ethyl acetate, vortex for 10 min, centrifuge at 12,000 rpm for 10 min at 4°C, transfer 850 µL of supernatant to a freshly labeled EP tube, concentrate in vacuo at 40°C for 45 min, add 100 µL of dichloromethane, and vortex to mix Evenly, it is made into plasma bambuterol extract.

[0053] 2. On-line combined detect...

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Abstract

The invention discloses an online microwave-assisted chiral derivatization-LC / MS (liquid chromatography / mass spectrometry) analysis system. The system comprises an online microwave assisted chiral derivatization device and an LC-MS device, wherein the online microwave assisted chiral derivatization device comprises a first chromatography pump, an automatic sample injector, a two-way mixer and a microwave synthesizer; acetonitrile pushed by the first chromatography pump flows through the automatic sample injector, the two-way mixer and a reaction tube of the microwave synthesizer sequentially; the LC-MS device comprises a second chromatography pump, a third chromatography pump, a six-way switching valve, a three-way micro-mixer, a chromatographic column and a mass spectrometry detector. The invention further provides an online microwave-assisted chiral derivatization-LC / MS analysis method based on the device. The device integrates mixing, reaction, separation and detection, mechanical drive and software control are adopted in the whole process, errors caused by manual operation can be reduced, and the precision and the accuracy of the method are greatly improved.

Description

technical field [0001] The invention relates to the field of sample processing for analyzing chiral compounds, in particular to an online microwave-assisted chiral derivatization-liquid mass spectrometry analysis system and method. Background technique [0002] Ultra Performance Liquid Chromatography\UPLC is a new category in separation science. It is faster and more sensitive than HPLC. It uses small particle column fillers, very low system volume and rapid detection New technologies such as means can obtain higher column efficiency and keep the column efficiency constant in a wider linear velocity range, which is beneficial to improve mobile phase flow rate, sensitivity, save analysis time and increase peak capacity. Moreover, its super strong separation ability also helps the separation of the target compound and the impurities that compete with it for ionization, so that the sensitivity of the detector can be further improved due to the weakening or overcoming of the ion...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027G01N2030/067
Inventor 周婷曾晶谭文赵婷
Owner SOUTH CHINA UNIV OF TECH
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