Hot phosphate-buffered water extraction coupled on-line with liquid chromatography/mass spectrometry for analyzing...

We evaluated the feasibility of analyzing rapidly traces of polar and medium polar contaminants in soil by coupling on-line a hot phosphate-buffered water extraction apparatus to a liquid chromatography/mass spectrometer system. Coupling was accomplished by using a small C-18 sorbent trap for collecting analytes and two six-port valves. The efficiency of this device was evaluated by extracting 13 selected pesticides from 200 mg of laboratory-aged soils by varying the extraction temperature, the extractant volume, and the flow rate at which the extractant passed through the extraction cell and the sorbent trap. In terms of extraction efficiency, robustness of the method, and extraction time, the best compromise was that of using 8 mL of extractant at 90 degrees C and 0.5 mL/min flow rate. Under these conditions, recoveries of 11 out of 13 analytes ranged between 82 and 103%, while those of the least hydrophilic pesticides, i.e., neburon and prochloraz, were 73 and 63%, respectively. By increasing the extractant volume to 60 mL, additional amounts of the two latter compounds could be recovered. Under this condition, however, the most hydrophilic analytes were in part no more retained by the C-18 sorbent trap. From a naturally 1.5-year aged soil, hot phosphate-buffered water removed larger amounts of three herbicides and hydroxyterbuthylazine (a terbuthylazine degradation product) than pure water and Soxhlet extraction. This result seems to confirm that hot phosphate buffer is also able to remove from soil those fractions of contaminants that, on aging, are sequestered into the humic acid framework.