DETERMINATION AND STABILITY OF PHENMEDIPHAN, ETHOFUMESATE AND FENAMIPHOS IN-GROUND WATER SAMPLES USING AUTOMATED SOLID-PHASE EXTRACTION CARTRIDGES FOLLOWED BY LIQUID-CHROMATOGRAPHY HIGH-FLOW PNEUMATICALLY ASSISTED ELECTROSPRAY MASS-SPECTROMETRY
C. Molina et al., DETERMINATION AND STABILITY OF PHENMEDIPHAN, ETHOFUMESATE AND FENAMIPHOS IN-GROUND WATER SAMPLES USING AUTOMATED SOLID-PHASE EXTRACTION CARTRIDGES FOLLOWED BY LIQUID-CHROMATOGRAPHY HIGH-FLOW PNEUMATICALLY ASSISTED ELECTROSPRAY MASS-SPECTROMETRY, International journal of environmental analytical chemistry, 65(1-4), 1996, pp. 69-82
The determination and stability of polar pesticides phenmediphan, etho
fumesate and fenamiphos in ground water samples was subjected to analy
sis with solid phase extraction (SPE) followed by liquid chromatograph
y-high flow pneumatically assisted electrospray mass spectrometry (LC-
ESP-MS). Pesticides were spiked at 6 mu g/L in ground water samples an
d 80 mt were preconcentrated by using an Automated Sample Preparation
with Extraction Columns (ASPEC XL) system. After preconcentration, sev
eral different storage conditions were tested, which included storage
at 4 degrees C, at -20 degrees C and at room temperature using styrene
divinylbenzene (SDB) cartridges. The percentage of degradation varied
from 20 to 80% for all the studied pesticides after 20 days of storag
e at room temperature. Phenmediphan and ethofumesate were stable at 4
degrees C and -20 degrees C during all the studied period whereas fena
miphos was recovered only 32 and 50% at 4 degrees C and -20 degrees C,
respectively, after 80 days of storage. The L.O.D under LC-ESP-MS and
SIM conditions were between 10-20 pg, 5-60 times lower as compared to
LC-thermospray-MS with no thermal degradation of phenmediphan. This h
igher sensitivity of LC-ESP-MS permitted the determination of fenamiph
os sulphoxide formed during the extraction and storage and the identif
ication of the interferences present in the cartridges e. g., diethyl
and di-n-butyl phthalates.