A. Martinesteban et al., PREPARATION, HOMOGENEITY AND STABILITY OF POLAR PESTICIDES IN FREEZE-DRIED WATER INTERLABORATORY EXERCISE, International journal of environmental analytical chemistry, 67(1-4), 1997, pp. 125-141
An interlaboratory exercise was carried out to improve the state of th
e art of some polar pesticide determination in water (atrazine, simazi
ne, carbaryl, propanil, linuron, fenamiphos and permethrin). The prepa
ration, the homogeneity and the stability of freeze-dried water sample
s containing the above pesticides was studied. The final concentration
of each pesticide in water was in the 50-80 mu g.l(-1) range with a s
alt content of 2.5 g.l(-1) of NaCl. After the lyophilization the resid
ue was rehomogenised, filled into amber glass bottles and stored at -2
0 degrees C and +20 degrees C. Every three months, one sample was anal
ysed to verify the stability of the residue. All pesticides were deter
mined by high performance liquid chromatography with diode-array detec
tion (HPLC-DAD) except permethrin which was determined by gas chromato
graphy with electron capture detection (GC-ECD). The results obtained
show that the atrazine, carbaryl, propanil, linuron and fenamiphos sam
ples were homogeneously distributed, whereas simazine and permethrin w
ere not. With respect to the stability over three months, all pesticid
es were stable at -20 degrees C. Atrazine, simazine, carbaryl, propani
l and linuron are also stable for the maximum storage time at +20 degr
ees C but the concentration of fenamiphos decreased by about 70% after
one month. The results obtained in the interlaboratory study by the p
articipants were in good agreement for many of the pesticides.