Solid phase dehydration extraction-supercritical fluid chromatography-mass spectrometry online analysis system and method
A supercritical fluid and analysis system technology, applied in the direction of analyzing materials, material separation, instruments, etc., can solve the problems that water-containing samples cannot be directly analyzed, and achieve the effect of improving separation effect, increasing polarity, and easy acquisition
Active Publication Date: 2021-11-02
SHIMADZU (CHINA) CO LTD +1
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Problems solved by technology
[0004] Based on this, the present invention aims to expand the analysis and application scope of supercritical fluid chromatography technology, overcome the shortcomings of supercritical fluid chromatography that cannot directly analyze water-containing samples, and overcome the problems in online extraction materials when online pretreatment technology is used in conjunction with supercritical fluid chromatography columns. The water will affect the separation effect of supercritical fluid chromatography, and overcome the difficulty of peak broadening caused by the large volume of strong desorption liquid entering the analytical column when the online pretreatment is directly desorbed before the column. Step, designed an online analysis system that can realize the analysis of aqueous samples through automatic extraction, dehydration, desorption, dilution, sample injection, and then the target can be separated and analyzed in the supercritical fluid chromatography-mass spectrometry system
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Embodiment 1
[0061] Using Waters HLB Oasis high-pressure column as the extraction column, 45 stimulants in human urine were analyzed using the solid phase dehydration extraction-supercritical fluid chromatography-mass spectrometry online analysis system.
[0062] The extraction column used in this method is Waters Oasis HLB direct connect HP column (20 μm particle size; 2.1 mm×30 mm), and the chromatographic column is Waters UPC2 Torus DIOL column (1.7 μm particle size, 2.1 mm×100 mm).
[0063] System connection and use such as Figure 1-5 shown. The autosampler 16 introduced 300 μL blank human urine spiked sample, and the first chromatographic pump 4 pushed pure water as the sample loading solution to send the urine sample into the Oasis HLB extraction column 13 . Then push the cleaning solution containing 5% acetonitrile aqueous solution into the Oasis HLB extraction column 13 for online impurity removal.
[0064] After the extraction is completed, switch the low-pressure six-way swit...
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The invention discloses a solid-phase dehydration extraction-supercritical fluid chromatography-mass spectrometry online analysis system, which includes an online enrichment-removal-cleaning device and an online dehydration-desorption-dilution-chromatographic separation device, and the device includes a carbon dioxide pump , three chromatographic pumps, two six-way switching valves, autosampler, extraction column, mixer, chromatographic column, three-way connector, mass spectrometer detector, through online enrichment-removal-cleaning device and online dehydration- The combination of desorption-dilution-chromatographic separation device realizes the online combination of supercritical fluid chromatography technology and pretreatment technology, enabling supercritical fluid chromatography technology to directly analyze aqueous samples. The entire analysis process is automatically controlled, with good chromatographic performance, high accuracy and precision, and can be effectively applied to the rapid analysis and detection of trace organic compounds in complex aqueous samples or aqueous extracts.
Description
technical field [0001] The invention belongs to the field of analytical chemical sample pretreatment, and specifically relates to a solid phase dehydration extraction-supercritical fluid chromatography-mass spectrometry online analysis system and method, which is suitable for trace amounts in liquid aqueous samples such as environment, food, medicine, biology, or liquid aqueous extracts On-line pretreatment, extraction, desorption, separation and detection of organic matter. Background technique [0002] Supercritical fluid chromatography (SFC) is a huge breakthrough in modern chromatographic technology. Because it has advantages that gas phase and liquid chromatography do not have, and can separate and analyze some objects that gas phase and liquid chromatography cannot solve, it is widely used , developed very rapidly. In SFC, the most widely used mobile phase is supercritical carbon dioxide, which is colorless, odorless, non-toxic, readily available and inexpensive, and ...
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IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/74
CPCG01N30/02G01N30/06G01N30/72G01N30/74G01N2030/027G01N2030/062
Inventor 刘佳琪周婷梁艳珊钟启升黄涛宏
Owner SHIMADZU (CHINA) CO LTD
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