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Method for analyzing short-chain chlorinated paraffin in environment sample by comprehensive two-dimensional gas chromatography-flight time mass spectrometry

A two-dimensional gas chromatography and time-of-flight mass spectrometry technology, applied in the field of analysis and testing, can solve the problems of lower recovery rate, increased risk of mixing other interference substances, and high detection cost

Active Publication Date: 2018-04-06
NAT RESERACH CENT OF GEOANALYSIS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method relies heavily on the chlorine content of SCCPs, and cannot detect SCCPs components with less than 5 chlorine atoms, and requires reactive gases, resulting in high detection costs
In addition, gas chromatography-subatomic bombardment-high resolution mass spectrometry (GC-MAB-HRMS), carbon skeleton gas chromatography, etc. can also be used for the detection of SCCPs, but due to the low popularity of equipment and complicated operation, the application is less
In short, in one-dimensional chromatography, SCCPs always appear as "finger-like" co-eluting peaks, and even if a high-resolution gas chromatography column is used, the homologues of SCCPs in the sample cannot be separated well
Moreover, since the retention time period of the characteristic peaks of SCCPs on the one-dimensional chromatogram is generally wide, other organic chlorides extracted at the same time as SCCPs will interfere with the analysis and detection of SCCPs and affect the accuracy of the results. Therefore, in order to ensure accurate determination, it is usually necessary to Adequate cleanup steps to separate or eliminate interferents from SCCPs
However, more purification steps tend to cause the loss of SCCPs in the sample, reduce the recovery rate, and increase the risk of mixing other interferences

Method used

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  • Method for analyzing short-chain chlorinated paraffin in environment sample by comprehensive two-dimensional gas chromatography-flight time mass spectrometry
  • Method for analyzing short-chain chlorinated paraffin in environment sample by comprehensive two-dimensional gas chromatography-flight time mass spectrometry
  • Method for analyzing short-chain chlorinated paraffin in environment sample by comprehensive two-dimensional gas chromatography-flight time mass spectrometry

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] The SCCPs standard solution (10.0 μg / mL) with a chlorination degree of 55.5% was drawn from the autosampler and injected into the gas chromatography-electron capture detector (GC-ECD) and the comprehensive two-dimensional gas chromatography-electron bombardment ionization source-low resolution Time-of-flight mass spectrometry (GC×GC-EI-TOF-LRMS) was used for detection, and the Figure 1A , 1B and 1C, Figure 1A : gas chromatography-electron capture detector method, Figure 1B : the inventive method (two-dimensional contour map), Figure 1C : the inventive method (three-dimensional stereogram).

[0080] In one-dimensional gas chromatography ( Figure 1A ), SCCPs present a "finger-like" coelution peak, and the coelution peak has a large retention time span, which is easily interfered by other peak substances in this area, and is not suitable for the determination of SCCPs in complex environmental samples. However, the separation effect of SCCPs by comprehensive two-di...

Embodiment 2

[0082] Using n-hexane as solvent, dilute step by step from 100 μg / mL standard solution of short-chain chlorinated paraffin (chlorination degree: 55.5%), and prepare the concentrations of 0.5, 1.0, 2.0, 5.0, 10.0 μg / mL containing 100 ng / mL The SCCPs series standard solutions were analyzed and tested according to the above experimental conditions. According to the peak area of ​​the molecular ion peak m / z89 shared by SCCPs and the internal standard substance, with the peak area ratio (=m / z 89 peak area / internal standard substance peak area) as the ordinate, the concentration ratio (=standard solution concentration / internal standard Concentration of standard substance) is the abscissa, and the standard curve is established, such as figure 2 shown. The functional relation of gained standard curve is y=0.0217x-0.0017, and wherein x represents the concentration ratio of SCCPs and internal standard substance, and y represents the peak area ratio of ∑ SCCPs and internal standard sub...

Embodiment 3

[0084] Qualitative experiment of SCCPs components by spectral library search and retention time index method. Select a soil sample and analyze it according to the process (steps 2 and 3) determined by this method. Then, using the same instrument method for C 8 -C 20 The standard solution was analyzed and tested. Afterwards, a data analysis method was established in the ChromaTOF software, and the one-dimensional chromatographic peak width was set to 18s, the two-dimensional chromatographic peak width was 0.1s, the signal-to-noise ratio was 50, and the standard spectral library was set to the NIST spectral library and contains SCCPs standard product information The self-built spectral library, the mass spectrum similarity is set to 600. Then, the method is used to automatically retrieve the samples, and after deducting the column loss and solvent residue, the information of each component of the sample is obtained, and the SCCPs components are preliminarily identified accord...

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Abstract

The invention discloses a method for analyzing short-chain chlorinated paraffin in an environment sample by a comprehensive two-dimensional gas chromatography-flight time mass spectrometry, which belongs to the technical field of analytical testing. The method comprises the following steps: 1) performing enrichment extraction on SCCPs in the environment sample; 2) employing a comprehensive two-dimensional gas chromatography-electron bombardment ionization source-low resolution time-of-flight mass spectrometer for detection; 3) employing library searching and a retention time index for determining the nature of the SCCPs component in the sample; and 4) employing an internal standard curve method for determining total amount of SCCPs. The pre-treatment method has the advantages of high extraction efficiency, good purifying effect, and wide application scope; the used apparatus has the advantages of high analysis efficiency, good separating effect, and strong anti-interference capability;the qualitative method is fast and accurate, and does not depend on a standard substance; the quantification method has the advantages of low detecting limit, low sensitivity, wide linearity range, and good repeatability, and the analysis requirement of SCCPs in the practical environment sample can be satisfied.

Description

technical field [0001] The invention relates to an analysis method for short-chain chlorinated paraffins in environmental samples, in particular to a method for analyzing short-chained chlorinated paraffins in environmental samples by comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry, and belongs to the technical field of analysis and testing. Background technique [0002] Short-chain chlorinated paraffins (Short-chain chlorinated paraffins, referred to as SCCPs), is a class of artificially synthesized chlorinated derivatives of normal alkanes, the carbon chain length is between 10-13 carbons, and the mass fraction of chlorine is usually between Between 30-72%. Due to the good industrial properties of SCCPs, as early as the 1930s, SCCPs were widely used in industrial products such as metal cutting fluids, sealants, adhesives, coatings, and flame retardants. However, studies have found that SCCPs are relatively stable in the environment, not e...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/06G01N30/08G01N30/86
CPCG01N30/02G01N30/06G01N30/08G01N30/72G01N30/8634G01N30/8696G01N2030/062
Inventor 战楠郭峰田芹饶竹
Owner NAT RESERACH CENT OF GEOANALYSIS
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