Does anyone have any experience of measuring PAHs from urine using GC-MS and any suggestions or published methods that may be helpful? Getting the full method is often very difficult from some papers.
According to the article “Determination of Urinary PAH Metabolites Using DLLME Hyphenated to Injector Port Silylation and GC–MS-MS “ a precise and eco-friendly analytical method has been developed for rapid determination of PAH metabolites. For the first time, a new analytical method based on coupling of dispersive liquid–liquid microextraction (DLLME) with auto-injector port silylation (auto-IPS) followed by gas chromatography–tandem mass spectrometry (GC–MS-MS) analysis is reported for the analysis of seven urinary PAH metabolites. Factors affecting DLLME and IPS, such as type and volume of extraction and disperser solvent, pH, ionic strength, injector port temperature, volume of N,O-bis(trimethylsilyl)trifluoroacetamide and type of solvent were investigated. Under optimized conditions, the limit of detection and limit of quantification were found to be in the range of 1–9 and 3–29 ng/mL, respectively. Satisfactory recoveries of metabolites in urine samples in the range of 87–95% were found.
As Mr. Ahmad, has properly underlined in his posting, the employment of standard GC-MS protocols yield to relatively low reliability of the analyses.
I would like to focus your attention on our own-authored (to me and my co-author's one as the papers have reflected) most recently developed stochastic dynamic mass spectrometric method and innovative model formulas for absolute quantification of analytes.
It has been tested on mixtures at pg.(mL)-1 and ng.(L)-1 concentration levels of the analytes. The linear correlation coefficients between theory and experiment are within /r/ = 0.99997 - 1. The method has been validated by chromatographic study, as well [1,2].
[1] Steroids, 164 (2020) 108750
Stochastic dynamic mass spectrometric quantification of steroids in mixture — Part II; Bojidarka Ivanova, Michael Spiteller
[2] B.Ivanova, M. Spiteller, Stochastic dynamic mass spectrometric approach to quantify reserpine in solution, (2020) in press.