Multi-Pesticide Analysis in Sediment by GC-EI-MS/MS Using Programmed Temperature Vaporization-Large Volume Injection Technique

A sensitive, selective and high throughput gas chromatography-tandem mass spectrometry method using programmable temperature vaporization-large volume injection mode (PTV-LVI-GC-MS/MS) for the analysis of 30 organochlorine pesticides (OCPs) including toxaphenes in sediments was developed. The PTV-LV injection settings, viz. inlet temperature, split flow, injection phase time, and injection speed were optimized for 50 A mu L injection. A significant increase in sensitivity was accomplished as compared with that obtained by the conventional 1 A mu L cold splitless injection. Average LVI recoveries for OCPs were in the range 58-133 % with low % RSD in instrument precision (< 12 %). The method detection limits achieved were 0.04-0.92 A mu g kg(-1). The method recovery ranged from 80 to 120 % with < 10 % RSD for more than 83 % of targeted analytes fortified at 10 A mu g kg(-1) in sediments. The PTV-LVI-GC-MS/MS allows simultaneous determination and unambiguous confirmation of trace OCPs and toxaphene congeners, which significantly streamlines and improves the trace organic analysis in the environmental surveillance and monitoring.