140
Additionally, a Varian triple quadrupole mass spectrometer (Wallnut Creek, USA) was
used. Gas chromatographic separations were carried out on a CP-3800 gas
chromatograph (Varian, Wallnut Creek, USA) applying a capillary of 15 m length and
0.25 mm ID coated with a film of 0.25 pm DB5-MS (5 % phenyl-methylpolysiloxane,
J&W Scientific, Folsom, USA). An injector temperature of 275 °C and Helium as
carrier gas (flow 2 ml/min) were used. The temperature programme was as follows: 100
°C for 1 min, then with 50 °C/min to 300 °C, isothermal for 4 min. Splitless injections
(splitless time 1.5 min) of 2.5 pi sample volume were carried with a Pal autosampler
(CTC Analytics, Zwingen, Switzerland).
The following EI-MS/MS conditions were applied: Electron energy 70 eV, filament
current 300 pA, resolution of quadrupole 1 at 0.8 u and of quadrupole 3 at 1.2 u, Ar as
collision gas at a pressure of 0.12-0.15 Pa (0.9-1.1 mTorr). The selected ions to be
fragmented as well as further parameters are given in Table 44. The precursor ion m/z
383 [M-C1] + and the product ion m/z 276 [M-4C1] + were selected for the internal
standard 1 ’Cio-/ra/7.s'-chlordane (collision energy -21 V).
Table 44: Selected precursor and product ions for the determination of the total PCA content by EI-
MS/MS with an ion trap and triple quadrupole mass spectrometer. Important instrument parameters and
the masses for the internal standard 13 Ci 0 -fran.s-chlordane are also given.
Precursor ion
(m/z)
Product ion
(m/z)
Ion trap
Triple quadrupole
Excitation am
plitude (V)
Excitation “storage
level” (m/z)
Collision energy
(V)
91 [C 7 H V ] +
53 [C 4 H 5 ] +
2,0
39,9
-16,0
102 [C 5 H 7 C1] +
65 [C 5 H 5 ] +
0,6
44,7
-10,0
102 [C 5 H 7 C1] +
67 [C 5 H 7 ] +
*
*
-18,0
383 [M-ClT
276 [M-4C1] +
0,85
169,0
-21,0
*not detectable in the ion trap.
5.6.9 Quantification of chlordanes by ECNI-LRMS
Gas chromatographic separations were carried out on an HP 5890II gas chromatograph
(Hewlett Packard, Palo Alto, USA), equipped with a Hewlett Packard 7673 auto
sampler. A fused silica capillary was employed of 15 m length and 0.25 mm ID coated