Novel chlorine-enhanced ionization reagent for liquid chromatography-mass spectrometry detection and application thereof
A liquid chromatography and mass spectrometry detection technology, which is applied in the field of chlorinated paraffin detection, can solve the problems of mass spectrometry or liquid phase system corrosion, ammonium chloride is not recommended, etc., to improve sensitivity and selectivity, improve sensitivity, and optimize chromatographic conditions Effect
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Embodiment 1
[0034] Such as Figure 1-2 As shown, the detection of CPs content in soil is as follows:
[0035] (1) Sample pretreatment
[0036] Take 5g soil sample, add 1g activated copper powder and 2g diatomaceous earth, add 20mL extractant (n-hexane-dichloromethane, volume ratio 1:1), vortex, ultrasonically extract for 20min, centrifuge (5000r / min, 5min) , take the supernatant. The residue was ultrasonically extracted twice with 2×10mL extractant, and the supernatants were combined. Blow the extraction liquid nitrogen to 1 mL, pass through an acidic silica gel column (concentrated sulfuric acid-silica gel, mass ratio 1:2), rinse with 10 mL n-hexane-dichloromethane (volume ratio 1:1), collect the eluate, and blow it with nitrogen to Dry, 500μL methanol to volume, to be detected by the instrument.
[0037] This is the extraction method recommended in this example, and other conventional extraction methods are also acceptable, as long as the chlorinated paraffin in the sample can be fu...
Embodiment 2
[0057] Such as Figure 1-2 As shown, the detection process of CPs content in chicken is as follows:
[0058] Take 2g chicken sample, add 20mL extractant (n-hexane-dichloromethane, volume ratio 1:1), vortex, ultrasonically extract for 20min, centrifuge (5000r / min, 5min), and take the supernatant. The residue was ultrasonically extracted twice with 2×10mL extractant, and the supernatants were combined. Blow the extraction liquid nitrogen to 1 mL, pass through an acidic silica gel column (concentrated sulfuric acid-silica gel, mass ratio 1:2), rinse with 10 mL n-hexane-dichloromethane (volume ratio 1:1), collect the eluate, and blow it with nitrogen to Dry, 500μL methanol to volume, to be detected by the instrument.
[0059] This is the extraction method recommended in this example, and other conventional extraction methods are also acceptable, as long as the chlorinated paraffin in the sample can be fully extracted.
[0060] The instrument conditions are the same as in Exampl...
Embodiment 3
[0067] The difference from Example 1 is that the concentration of tetramethylammonium chloride is 0.08mM.
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