Organophosphonate Degradation Product Analysis via UHPLC-MS/MS by PHILIS Mobile Laboratory for High Throughput Emergency Response Field Operations

Oral Presentation

Prepared by J. Capri1, J. Garcia1, A. Gugliotta1, A. Bleich1, L. Kaelin2, T. Smith3
1 - CSS-Dynamac Corporation, 8833 Cincinnati Dayton Road, Suite 202, West Chester , OH, 45069, United States
2 - US EPA OEM, 2890 Woodbridge Ave, Edison, NJ, 08837, United States
3 - US EPA OEM, William Jefferson Clinton Building, 1200 Pennsylvania Avenue, N.W. MC 5104A, Washington, DC, 20460, United States


Contact Information: [email protected]; 513-708-5982


ABSTRACT

The Portable High Throughput Integrated Laboratory Identification System or “PHILIS” are NELAP accredited mobile laboratories that were designed to provide real-time, on-site analytical data for emergency response and other environmental investigation projects under the direction of the US EPA Office of Emergency Management. PHILIS mobile laboratory operations are housed in nine uniquely configured vehicles that are maintained at base operations located in New Jersey and Colorado.

A fast, reliable method for the analysis of organophosphonate (nerve agent) degradation products was developed using UPLC-MS/MS in the PHILIS Performance Analytical Laboratory (PAL) mobile lab unit, stationed in Castle Rock, CO. This method is suitable for water, soil and wipe samples, following the appropriate extraction steps, without the need for derivatization. The analysis is performed using a hydrophilic interaction chromatography (HILIC) technique. The total cycle time for nine analytes was less than seven minutes, providing capability to analyze 120 samples per 24 hour clock. Average recoveries for the degradation products ranged from 73% to 125%, and MDL values were less than 20 µg/L for waters, 20 to 65 µg/kg for soil samples, and less than 10 ng per wipe sample.

For the mobile laboratory operation, water and wipe samples were prepared using a micro-extraction procedure. Soil samples were prepared using pressurized sample extraction. Procedures were validated to ensure that analysis meets recovery and reporting limit requirements. Mobile labs do not have adequate space for traditional procedures, such as liquid-liquid extractors. Items such as dedicated refrigerators must be available for standards, extracts, and sample storage, requiring project coordination for sample sizes and quantity. Special hardware, such as vibration dampers and inertia and isolation mounts are used to protect and maintain sensitive equipment during mobile laboratory operations.