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On-line analysis system for automatic pretreatment by adopting ultra high performance liquid chromatography/mass spectrum

An ultra-high performance liquid chromatography and analysis system technology, which is applied in the field of automatic pretreatment - ultra-high performance liquid chromatography/mass spectrometry online analysis system to broaden the applicability and application scope of the system, improve the precision and accuracy of the method, and achieve a high degree of automation Effect

Active Publication Date: 2014-07-23
SHIMADZU (CHINA) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims to overcome the disadvantages that atmospheric pressure extraction materials cannot withstand the pressure of ultra-high performance liquid chromatography for direct pre-column desorption, the disadvantages of peak broadening after sample injection of large-volume strong solvent desorption liquid, and the need for liquid chromatography-mass spectrometry Using the special requirements of the post-column compensation liquid, an online analysis system that can realize the automatic extraction, desorption, and injection of liquid samples through atmospheric extraction materials, and then allow the target substances to be separated and analyzed by ultra-high performance liquid chromatography-mass spectrometer

Method used

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  • On-line analysis system for automatic pretreatment by adopting ultra high performance liquid chromatography/mass spectrum
  • On-line analysis system for automatic pretreatment by adopting ultra high performance liquid chromatography/mass spectrum
  • On-line analysis system for automatic pretreatment by adopting ultra high performance liquid chromatography/mass spectrum

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Experimental program
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Effect test

Embodiment 1

[0060] Using the Shimadzu MAYI-SAX column as the extraction column, the three auxins in the plant extract were analyzed by using the automatic pretreatment-ultra high performance liquid chromatography / mass spectrometry online analysis system automatic pretreatment mode.

[0061] The extraction column used in this method is Shimadzu Shim-pack MAYI-SAX (G) 10L×4.6, and the chromatographic column is Shimadzu Shim-pack XR-ODS III, 2.0mm×50mm L (1.6μm particle size).

[0062] Combined flow path such as figure 1 shown.

[0063] The autosampler 5 introduces 50 μL of the spiked plant extract sample, and the first chromatographic pump 1 pushes a 0.01mol ammonium acetate / acetonitrile (95 / 5, v / v) sample loading solution to send the sample into the online diluter 6, Then the diluted sample enters the MAYI-SAX extraction column 7 for online extraction; after the extraction is completed, the first high-pressure six-way switching valve 8 is switched, and the MAYI-SAX extraction column 7 is ...

Embodiment 2

[0066] The post-column compensation mode of the automatic pretreatment-ultra high performance liquid chromatography / mass spectrometry online analysis system was used to evaluate the matrix effect of the bamboo leaf samples.

[0067] On the basis of the automatic pretreatment mode, the system has undergone the following modification, which can facilitate the post-column compensation analysis: disconnect the direct connection pipe between the three-way 14 and the third high-pressure six-way switching valve 18, inject the solution with the syringe 17 to fill the second The sample loop 16 is connected directly to the tee 14 and the third high-pressure six-way switching valve 18 for post-column compensation analysis. The extraction column used in this method is Shimadzu Shim-pack MAYI-SAX (G) 10L×4.6, the chromatographic column is Shimadzu Shim-pack XR-ODS III, 2.0mm×50mm L (1.6μm particle size), the second The sample loop is a 1mL stainless steel loop.

[0068] Combined flow path...

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Abstract

The invention discloses an on-line analysis system for automatic pretreatment by adopting an ultra-high performance liquid chromatography / mass spectrum. The on-line analysis system has an automatic pretreatment mode and a post-column compensation mode, and comprises four chromatography pumps, two high-pressure switch valves, an automatic sample injector, an on-line diluter, an extraction column, an on-line filter, two sample rings, a miniature mixer, a chromatographic column, a tee joint, a mass spectrometry detector and the like. On-line dilution, extraction, desorption, separation, detection and post-column compensation analysis can be carried out on a target analyte in a liquid sample by combination of an on-line dilution / extraction / desorption device, a stigma focusing device, a post-column compensation device and an ultra high performance liquid chromatography / mass spectrum device, the overall analysis process is automatically controlled, and is high in accuracy and precision, and the on-line analysis system can be effectively applied to the analysis detection on trace organic compounds in a complicated liquid sample or a liquid extracting solution.

Description

technical field [0001] The invention belongs to the field of analytical chemical sample pretreatment, and in particular relates to the design, analysis and application of an automatic pretreatment-ultra high performance liquid chromatography / mass spectrometry online analysis system, which is suitable for liquid samples or liquid extractions such as the environment, food, medicine, and biology On-line pretreatment, extraction, desorption, separation and detection of trace organic matter in liquid. Background technique [0002] Ultra High Performance Liquid Chromatography (UHPLC) is a huge breakthrough in liquid chromatography technology and the development trend of modern separation analysis. UHPLC achieves higher column efficiency by reducing the particle size of the stationary phase filler and smaller inner diameter chromatographic column, and reduces the analysis time by shortening the length of the chromatographic column, so the analysis speed of UHPLC can usually reach s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 钟启升林才勇邱雄雄申玲玲霍茵詹松姚劲挺黄涛宏
Owner SHIMADZU (CHINA) CO LTD
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