PMID- 29909622 OWN - NLM STAT- PubMed-not-MEDLINE DCOM- 20190313 LR - 20190313 IS - 1520-6882 (Electronic) IS - 0003-2700 (Linking) VI - 90 IP - 14 DP - 2018 Jul 17 TI - Efficient Extraction of Sulfur and Nitrogen Mustards from Nonpolar Matrix and an Investigation on Their Sorption Behavior on Silica. PG - 8295-8299 LID - 10.1021/acs.analchem.8b02157 [doi] AB - Extraction of vesicant class of chemical warfare agents (CWAs) such as sulfur mustard and nitrogen mustards from the environmental matrices is of prime importance, from a forensic and verification viewpoint of the Chemical Weapons Convention (CWC). For extraction of Convention Related Compounds from nonpolar organic medium, commercially available silica cartridges are used extensively, but silica cartridges exhibit limited efficiency toward vesicant classes of compounds. It is expected that sulfur mustard being nonpolar does not retain sufficiently on silica surface, and nitrogen mustards (being basic) are strongly adsorbed on acidic silica surface, resulting in their poor recoveries. Contrary to the expected higher recovery of sulfur mustard over nitrogen mustards, it was observed that the recovery of sulfur mustard was lower than that of nitrogen mustards with the silica based sorbent. The reason for this typical behavior of these agents on silica was investigated. This study was aimed to develop an analytical method for efficient extraction and enrichment of sulfur and nitrogen mustards from hydrophobic matrices. In this work, the polymeric sorbent was synthesized with polar methacrylic acid (MAA) as monomer and ethylene glycol dimethacrylate (EGDMA) as cross-linker and used for solid phase extraction (SPE) of sulfur mustard and nitrogen mustards. The extraction efficiency of the polymeric sorbent was optimized and compared with that of silica cartridges. Both classes of analytes were recovered in good amounts from the polymeric sorbent compared to silica. The extraction parameters were optimized for the proposed method which included extraction solvent ethyl acetate and washing solvent n-hexane (1 mL). The recoveries of the analytes ranged from 75 to 87% with relative standard deviations (RSDs) lower than 9%. The limit of detection (LOD) was found to be in the range of 0.075-0.150 mug mL(-1), and limit of quantification (LOQ) was >0.25 mug mL(-1). The linear dynamic range of optimized method was found to be 0.50-20 mug mL(-1) ( r(2) = 0.9994) for sulfur mustard and 0.25-20 mug mL(-1) ( r(2) = 0.9897-0.9987) for nitrogen mustards, respectively. FAU - Sinha Roy, Kanchan AU - Sinha Roy K AUID- ORCID: 0000-0001-7726-6788 AD - VERTOX Laboratory , Defence Research and Development Establishment , Jhansi Road , Gwalior 474002 , Madhya Pradesh , India. FAU - Goud, D Raghavender AU - Goud DR AD - VERTOX Laboratory , Defence Research and Development Establishment , Jhansi Road , Gwalior 474002 , Madhya Pradesh , India. FAU - Chandra, Buddhadeb AU - Chandra B AUID- ORCID: 0000-0003-0146-8804 AD - VERTOX Laboratory , Defence Research and Development Establishment , Jhansi Road , Gwalior 474002 , Madhya Pradesh , India. FAU - Dubey, Devendra Kumar AU - Dubey DK AUID- ORCID: 0000-0003-3820-2233 AD - VERTOX Laboratory , Defence Research and Development Establishment , Jhansi Road , Gwalior 474002 , Madhya Pradesh , India. LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20180627 PL - United States TA - Anal Chem JT - Analytical chemistry JID - 0370536 EDAT- 2018/06/19 06:00 MHDA- 2018/06/19 06:01 CRDT- 2018/06/19 06:00 PHST- 2018/06/19 06:00 [pubmed] PHST- 2018/06/19 06:01 [medline] PHST- 2018/06/19 06:00 [entrez] AID - 10.1021/acs.analchem.8b02157 [doi] PST - ppublish SO - Anal Chem. 2018 Jul 17;90(14):8295-8299. doi: 10.1021/acs.analchem.8b02157. Epub 2018 Jun 27.