PMID- 35791603 OWN - NLM STAT- MEDLINE DCOM- 20220707 LR - 20220915 IS - 1872-2059 (Electronic) IS - 1000-8713 (Print) IS - 1000-8713 (Linking) VI - 40 IP - 7 DP - 2022 Jul TI - [Determination of polychlorinated naphthalenes in ambient air by isotope dilution gas chromatography-triple quadrupole mass spectrometry]. PG - 644-652 LID - 10.3724/SP.J.1123.2021.12006 [doi] AB - Polychlorinated naphthalenes (PCNs) have a structure similar to that of polychlorinated biphenyls (PCBs) and represent a new type of persistent organic pollutants (POPs) that are widely present in the environment and biological communities. PCNs can migrate and transform via different environmental media, which severely affects the health of humans and organisms. Researchers have devoted considerable focus on ambient air pollution. Although the current ambient air quality has not yet limited the concentration of PCNs, the Stockholm Convention has required parties to prohibit and eliminate their production and use. As one of the contracting parties, China is obligated to improve its environmental monitoring. In other words, the development of a method for monitoring PCNs in ambient air is important for understanding ambient air quality and safeguarding human health. PCNs are generally present at trace levels (pg/m(3)) in ambient air. To achieve accurate quantification of PCNs, high demands are raised on the methods for extraction, purification, and instrumental analysis, which can directly affect the efficiency, accuracy, and sensitivity of a method. Considering the trace-level presence of PCNs in ambient air and the high efficiency and accuracy of the analytical method, accelerated solvent extraction (ASE), combined with column chromatography using a multilayer silica gel column and a neutral alumina column, was established for the extraction and purification of PCNs in ambient air. The important parameters involved in the aforementioned steps, such as the type of extraction and volume of elution solvent, were optimized. The results indicated that dichloromethane-hexane (1ratio1, v/v) was the best extraction solvent for the recovery of PCNs. Hexane and dichloromethane-hexane (5ratio95, v/v) were used as the elution solvents for the multi-silica gel column and neutral alumina column, respectively. Isotope dilution gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) was used to quantify the target compounds. Gas chromatographic parameters, such as temperature program conditions and inlet temperature, were also optimized. The oven temperature program was as follows: 80 ℃ for 1 min, 80 ℃ to 160 ℃ at 15 ℃/min, 160 ℃ to 265 ℃ at 3 ℃/min, and 265 ℃ to 280 ℃ at 5 ℃/min, followed by holding the temperature at 280 ℃ for 10 min. The inlet temperature was set at 260 ℃. The optimal characteristics of ion pair, collision energy, and ion source temperature were determined by optimizing the key mass spectrometry parameters. The developed instrumental method, combined with suitable sample preparation techniques, was used to determine the concentrations of PCNs in ambient air samples. Quality control (QC) and quality assurance (QA) were performed by adding isotope internal standards before sampling, extraction, and injection analysis to monitor the entire analysis process. The relative standard deviations (RSDs) of the relative response factors (RRFs) for trichloronaphthalene to octachloronaphthalene were less than 16% in the concentration range of 2-100 ng/mL. The method detection limits (MDLs) for PCN homologues were in the range of 1-3 pg/m(3)(calculated using a sample volume of 288 m(3)). The precision and accuracy of this method for determining PCNs in ambient air samples were evaluated using a spiked matrix. The average spiked recoveries of trichloronaphthalene to octachloronaphthalene were 89.0%-119.4%, 98.6%-122.5% and 93.7%-124.5% at low, medium, and high spiked concentrations (20, 50, and 90 ng/mL), respectively. The RSDs of the assay results were 1.9%-7.0%, 1.6%-6.6%, and 1.0%-4.8%, respectively. During the entire analysis process, the average recoveries of the sampling and extracted internal standards were 136.2%-146.0% and 42.4%-78.1%, respectively, and the corresponding RSDs were 5.6%-7.5% and 2.7%-17.5%. Thus, this method meets the requirements of trace analysis and exhibits good parallelism, high sensitivity, high accuracy, and good precision, and it is suitable for the accurate quantitative determination of trichloronaphthalene to octachloronaphthalene in ambient air. FAU - Liu, Hongyuan AU - Liu H AD - Shenyang Pharmaceutical University, Shenyang 110000, China. AD - CAS Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China. FAU - Jin, Jing AU - Jin J AD - CAS Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China. FAU - Guo, Cuicui AU - Guo C AD - CAS Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China. AD - University of Chinese Academy of Sciences, Beijing 100012, China. FAU - Chen, Jiping AU - Chen J AD - CAS Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China. FAU - Hu, Chun AU - Hu C AD - Shenyang Pharmaceutical University, Shenyang 110000, China. LA - chi PT - Journal Article PL - China TA - Se Pu JT - Se pu = Chinese journal of chromatography JID - 9424804 RN - 0 (Hexanes) RN - 0 (Isotopes) RN - 0 (Naphthalenes) RN - 0 (Solvents) RN - 588X2YUY0A (Methylene Chloride) RN - 60650-90-0 (Silica Gel) RN - LMI26O6933 (Aluminum Oxide) SB - IM MH - Aluminum Oxide MH - Gas Chromatography-Mass Spectrometry/methods MH - *Hexanes/analysis MH - Humans MH - Isotopes MH - Methylene Chloride/analysis MH - *Naphthalenes/analysis MH - Silica Gel MH - Solvents/analysis MH - Tandem Mass Spectrometry/methods PMC - PMC9404119 OTO - NOTNLM OT - ambient air OT - gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) OT - isotope dilution OT - polychlorinated naphthalenes (PCNs) EDAT- 2022/07/07 06:00 MHDA- 2022/07/08 06:00 PMCR- 2022/07/08 CRDT- 2022/07/06 03:02 PHST- 2022/07/06 03:02 [entrez] PHST- 2022/07/07 06:00 [pubmed] PHST- 2022/07/08 06:00 [medline] PHST- 2022/07/08 00:00 [pmc-release] AID - 10.3724/SP.J.1123.2021.12006 [doi] PST - ppublish SO - Se Pu. 2022 Jul;40(7):644-652. doi: 10.3724/SP.J.1123.2021.12006.