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
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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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