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Pesticide residues
Figure 2.8.12.-2
Introduce into the flask the prescribed quantity of the drug
and continue the distillation as described above for the
time and at the rate prescribed. Stop the heating and after
10 min read the volume of liquid collected in the graduated
tube and subtract the volume of xylene previously noted.
The difference represents the quantity of essential oil in the
mass of the drug taken. Calculate the result as millilitres
per kilogram of drug.
When the essential oil is to be used for other analytical
purposes, the water-free mixture of xylene and essential
oil may be recovered as follows : remove the stopper K
and introduce 0.1 ml of a 1 g/l solution of sodium
fluoresceinate R and 0.5 ml of water R. Lower the mixture
of xylene and essential oil into the bulb-shaped swelling L
by means of the three-way tap, allow to stand for 5 min and
lower the mixture slowly until it just reaches the level of the
tap M. Open the tap anti-clockwise so that the water flows out
of the connecting tube BM. Wash the tube with acetone R
and with a little toluene R introduced through the filling
funnel N. Turn the tap anti-clockwise in order to recover the
mixture of xylene and essential oil in an appropriate flask.
219
Table 2.8.13.-3
Substance
Dichlorvos
0.20
Fonofos
0.50
Diazinon
0.52
Parathion-methyl
0.59
Chlorpyrifos-methyl
0.60
Pirimiphos-methyl
0.66
Malathion
0.67
Parathion
0.69
Chlorpyrifos
0.70
Methidathion
0.78
Ethion
0.96
Carbophenothion
1.00
Azinphos-methyl
1.17
Phosalon
1.18
Test solution. Concentrate solution B in a current of helium The chromatographic procedure may be carried out using :
for chromatography R almost to dryness and dilute to 100 l a fused silica column 30 m long and 0.32 mm in internal
diameter the internal wall of which is covered with a layer
with toluene R.
0.25 m thick of poly(dimethyl)(diphenyl)siloxane R,
Reference solution. Prepare at least three solutions in
hydrogen for chromatography R as the carrier gas. Other
toluene R containing the insecticides to be determined and
gases such as helium for chromatography R or nitrogen
carbophenothion at concentrations suitable for plotting a
for chromatography R may also be used, provided the
calibration curve.
chromatography is suitably validated,
an
electron-capture detector,
The chromatographic procedure may be carried out using :
a device allowing direct cold on-column injection,
a fused-silica column 30 m long and 0.32 mm in internal maintaining the temperature of the column at 80 C for
diameter the internal wall of which is covered with a layer 1 min, then raising it at a rate of 30 C/min to 150 C,
0.25 m thick of poly(dimethyl)siloxane R,
maintaining at 150 C for 3 min, then raising the temperature
hydrogen for chromatography R as the carrier gas. Other at a rate of 4 C/min to 280 C and maintaining at this
gases such as helium for chromatography R or nitrogen temperature for 1 min, and maintaining the temperature
of the injector port at 250 C and that of the detector at
for chromatography R may also be used provided the
275 C. Inject the chosen volume of each solution. When the
chromatography is suitably validated.
chromatograms are recorded in the prescribed conditions,
the relative retention times are approximately those listed
a phosphorus-nitrogen flame-ionisation detector or a
in Table 2.8.13.-4. Calculate the content of each insecticide
atomic emission spectrometry detector,
from the peak areas and the concentrations of the solutions.
maintaining the temperature of the column at 80 C for
Table 2.8.13.-4
1 min, then raising it at a rate of 30 C/min to 150 C,
Relative rentention times
maintaining at 150 C for 3 min, then raising the temperature Substance
at a rate of 4 C/min to 280 C and maintaining at this
0.44
-Hexachlorocyclohexane
temperature for 1 min, and maintaining the temperature
0.45
Hexachlorobenzene
of the injector port at 250 C and that of the detector at
275 C. Inject the chosen volume of each solution. When the -Hexachlorocyclohexane
0.49
chromatograms are recorded in the prescribed conditions,
0.49
Lindane
the relative retention times are approximately those listed
in Table 2.8.13.-3. Calculate the content of each insecticide
0.54
-Hexachlorocyclohexane
from the peak areas and the concentrations of the solutions.
3.2. Organochlorine and pyrethroid insecticides. Examine
by gas chromatography (2.2.28), using carbophenothion as
the internal standard. It may be necessary to use a second
internal standard to identify possible interference with the
peak corresponding to carbophenothion
Test solution. Concentrate solution C in a current of helium
for chromatography R or oxygen-free nitrogen R almost to
dryness and dilute to 500 l with toluene R.
Reference solution. Prepare at least three solutions in
toluene R containing the insecticides to be determined and
carbophenothion at concentrations suitable for plotting a
calibration curve.
220
-Hexachlorocyclohexane
0.56
Heptachlor
0.61
Aldrin
0.68
cis-Heptachlor-epoxide
0.76
o,p-DDE
0.81
-Endosulfan
0.82
Dieldrin
0.87
p,p-DDE
0.87
o,p-DDD
0.89
Endrin
0.91
Substance
01/2005:20815
-Endosulfan
0.92
o,p-DDT
0.95
1.00
m2