Determination of Emerging Contaminants in Wastewater Utilizing Comprehensive Two-Dimensional Gas-Chromatography Coupled with Time-of-Flight Mass Spectrometry

Author(s): Sarah Prebihalo1, Adrienne Brockman1, Jack Cochran1,2, Frank L. Dorman1,3

1. Pennsylvania State University, Forensic Science Program
2. Restek Corporation
3. Pennsylvania State University, Department of Biochemistry and Molecular Biology

Published By: Journal of Chromatography A

Year of Publication: 2015

Link: www.sciencedirect.com/science/article/pii/S0021967315014132

Abstract: An analytical method for identification of emerging contaminants of concern, such as pesticides and organohalogens has been developed and utilized for true discovery-based analysis. In order to achieve the level of sensitivity and selectivity necessary for detecting compounds in complex samples, comprehensive gas chromatography coupled with time-of-flight mass spectrometry (GCxGC-TOFMS) was utilized to analyze wastewater samples obtained from the Pennsylvania State University wastewater treatment facility (WWTF). Determination of emerging contaminants through a process of combining samples which represent “normal background” and comparing this to new samples was developed. Results show the presence of halogenated benzotriazoles in wastewater samples as well as soil samples from Pennsylvania State University agricultural fields. The trace levels of chlorinated benzotriazoles observed in the monitoring wells present on the property indicate likely environmental degradation of the chlorinated benzotriazoles. Preliminary investigation of environmental fate of the substituted benzotriazoles indicates their likely degradation into phenol; an Environmental Protection Agency (USEPA) priority pollutant.

Misselwitz and Rattray to Speak at the EPA’s 22nd Annual Quality Assurance Conference

Chris Rattray

Chris Rattray

Michelle Misselwitz

Michelle Misselwitz

From October 15–19, 2012, the U.S. Environmental Protection Agency (EPA) will hold its 22nd Annual Quality Assurance Conference in Region 6, Dallas, TX. Two Restek chemists, Michelle Misselwitz and Chris Rattray, will be making the trip south to present some of their latest work, including GCxGC analysis of pesticides and pharmaceutical and personal care products (PPCPs) as well as lowering detection limits for drinking water methods using large volume splitless injection (LVSI). For more details on each presentation, see below.

This free conference has been organized for years by the incredibly dedicated Charles Ritchie and is a great way to network with a wide range of colleagues and get caught up to speed on recent developments in environmental analysis. You can learn more about the Quality Assurance Conference on the EPA’s website (www.epa.gov/earth1r6/qa/index12.htm) and can also re-read Michelle Misselwitz’s blog on last year’s event (blog.restek.com/?p=3916) .

We hope to see you there!

 

Technical Presentations

TUESDAY, OCTOBER 16, 2012

9:30 a.m. / Session E
The QuEChERS Sample Preparation Approach and Comprehensive Two-Dimensional Gas Chromatography Time-of-Flight Mass Spectrometry for the Analysis of Pesticides in Tobacco

Michelle Misselwitz

Tobacco is a high-value production crop for the United States and ranks 6th among the amount of pesticides applied per acre in American agriculture. Even after the processing of tobacco, some pesticide residues remain on the final product. We used the Quick–Easy–Cheap–Effective–Rugged–Safe (QuEChERS) sample preparation approach to isolate pesticide residues from loose cigarette tobacco. Comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GCxGC-TOFMS) was used to determine pesticide residues in the resulting extracts.

3:00 p.m. / Session C
Analysis of Pharmaceutical and Personal Care Products and Other Emerging Environmental Contaminants in Water Using a Highly Efficient GCxGC-TOFMS System

Michelle Misselwitz

Comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GCxGC-TOFMS) is a powerful multidimensional approach to sample analysis that is unmatched by traditional one-dimensional chromatography. By operating the system to maximize efficiency in both the first and second dimension, GCxGC-TOFMS has the ability to detect, identify, and quantify or semi-quantify an unlimited number of target, non-target, and unknown compounds (including emerging compounds of concern) with full mass spectra and sub- to low-pg sensitivity. Using this technique, water samples were collected from the urban river in Las Vegas to analyze a large number of pharmaceutical and personal care products and other emerging environmental contaminants.

4:00 p.m. / Session D
Achieving Lower Detection Limits for Multiple Drinking Water Methods Using Large Volume Splitless Injections on an Unmodified Split/Splitless Injection Port

Chris Rattray
For more information, email Chris Rattray.

Utilizing a large volume splitless injection is advantageous for many reasons. Some of these include shipping and extracting significantly smaller sample sizes, reducing extract concentration, or decreasing limits of detection for trace-level analysis in drinking water. The drawback for many is that large volume injections typically require a specialized injection port. However, with concurrent solvent recondensation-large volume splitless injection (CSR-LVSI), a large volume injection can be achieved on an unmodified Agilent split/splitless injection port. Here we analyzed multiple drinking water methods using CSR-LVSI on an Agilent 7890/5975C GC-MSD and injected up to 10 µL to achieve lower detection limits.