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

Active Publication Date: 2021-01-22
广东省农业科学院农业质量标准与监测技术研究所
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AI Technical Summary

Problems solved by technology

However, since ammonium chloride provides chloride ions by decomposing into hydrogen chloride gas under the high temperature conditions of the ion source, hydrogen chloride has a strong corrosive effect on metals, so it is generally not recommended to use ammonium chloride in mass spectrometry
In summary, currently only the UPLC-HRMS method promoted by halogen-enhanced ionization reagents (dichloromethane, bromoform or ammonium chloride, etc.) can realize the simultaneous analysis of three CPs. However, the current halogen-enhanced ionization reagents Corrosive to MS or LC systems

Method used

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  • Novel chlorine-enhanced ionization reagent for liquid chromatography-mass spectrometry detection and application thereof
  • Novel chlorine-enhanced ionization reagent for liquid chromatography-mass spectrometry detection and application thereof
  • Novel chlorine-enhanced ionization reagent for liquid chromatography-mass spectrometry detection and application thereof

Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention discloses a novel chlorine-enhanced ionization reagent for liquid chromatography-mass spectrometry detection. The novel chlorine-enhanced ionization reagent is organic chlorine salt-tetramethylammonium chloride (TMAC) with volatility, and has no corrosion to a liquid chromatography system and a mass spectrometry system. The invention provides application of the chlorine-enhanced ionization reagent in liquid chromatography-high-resolution mass spectrometry detection of chlorinated paraffin, the result shows that TMAC is used as a mobile phase additive, the CPs detection sensitivity and selectivity can be remarkably improved under the condition of original configuration of an instrument, and the method is not influenced by the CPs carbon chain length and the chlorine content.

Description

technical field [0001] The invention belongs to the technical field of chlorinated paraffin detection, and in particular relates to a novel chlorine-enhanced ionization reagent for liquid chromatography-mass spectrometry detection and its application. Background technique [0002] Chlorinated paraffins (CPs) are one of the most serious halogenated organic pollutants (OHPs) in my country's environmental media and agricultural products. It is mainly used in the metal processing industry and the plastics industry. According to the carbon chain length, CPs commercial products are divided into short-chain chlorinated paraffins (SCCPs, C10-13), medium-chain chlorinated paraffins (MCCPs, C14-17) and long-chain chlorinated paraffins (LCCPs, C≥18). In recent years, international scholars have carried out in-depth research on the environmental media of SCCPs, the distribution characteristics of organisms and human bodies, migration and transformation, ecological / health toxicity, etc....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72
CPCG01N30/02G01N30/72G01N2030/042
Inventor 黄晓梅王旭王威利丁晨红殷秋妙王英苏秋权
Owner 广东省农业科学院农业质量标准与监测技术研究所
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