Citation: ZHOU Xi, WU Hui-Qin, HUANG Fang, HUANG Xiao-Lan, LIN Xiao-Shan, HOU Si-Run, LI Rong-Xi. Determination of Short Chain Chlorinated Paraffins in Plastic by High Performance Liquid Chromatography Coupled with Electron Spray Ionization Quadrupole Time-of-flight Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2019, 47(4): 519-526. doi: 10.19756/j.issn.0253-3820.181646 shu

Determination of Short Chain Chlorinated Paraffins in Plastic by High Performance Liquid Chromatography Coupled with Electron Spray Ionization Quadrupole Time-of-flight Mass Spectrometry

Guangdong Provincial Key Laboratory of Emergency Test for Dangerous Chemicals, Guangdong Provincial Public Laboratory of Analysis and Testing Technology, Guangdong Institute of Analysis, Guangzhou 510070, China

Received Date: 31 October 2018
Revised Date: 26 December 2018

Fund Project: This work was supported by the Provincial Innovative Talents Introduction Foundation of Guangdong, China (No. 2018GDASCX-0919).

A method of high performance liquid chromatography coupled with electron spray ionization quadrupole time-of-flight mass spectrometry was established for analysis of short chain chlorinated paraffins (SCCPs) in plastic. No chlorine solvent was added and SCCPs were quantified by their[M-H]^- ions. For each congener group of SCCPs with carbon chain lengths in 10-13 and chlorine substituents in 5-13, the two most abundant m/z signals were extracted from the full-scan mass spectra as the quantitative and qualitative ions. The influence of medium chain chlorinated paraffins (MCCPs) was eliminated efficiently based on the high resolution of the mass spectrometry. Plastic samples were extracted by dichloride methane and purified by silica gel solid phase extraction column. SCCPs were eluted by hexane/dichloride methane (1:1, V/V). The instrumental detection limits (IDLs) were 0.01-0.05 mg/L for SCCPs with chlorine content from 51.5%-63%. Method detection limit (MDL) and quantitative limit were 1.4 μg/g and 4.6 μg/g, respectively. Recoveries of SCCPs were 118.0%±8.2%, 81.9%±6.9% and 77.8%±6.6%, at spiking concentrations of 5 μg/g, 20 μg/g and 50 μg/g, respectively. The intra- and inter-day variations were 5.7% and 8.1%, respectively. The quantitative results verified that SCCPs concentration in CPs were similar with the short chain alkane in the corresponding paraffin, which demonstrated the accuracy of this method. This method was applied in determination of four kinds of plastic samples. Cable and track presented to have a high concentration of SCCPs within the range of 555-1049 μg/g. Plastic toys had lower concentrations of SCCPs in the range of 1.86-6.56 μg/g.
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