300920 Antineoplastic Agents from Sewage Water

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Antineoplastic Agents from Sewage Water

Summary

Type: SPE
Application #: 300920
Catalog#: 730003 - SPE Cartridges, Chromabond, C18, 3ml, PP, 500mg, 50/pk
Detection: GC
Conditions: Step 1:
Column conditioning:
3 ml hexane, 3 ml methanol, then 10 ml deionised water with 3 ml/min each

Sample application:
Force or aspirate the filtered sample through the column with 3 ml/min

Column washing:
10 ml deionised water with 3 ml/min; then evacuate the column, dry it under a
stream of nitrogen and finally wash with 500 μl hexane

Elution:
2 ml methanol / acetone (95:5, v/v); evaporate the eluate in a stream of
nitrogen and redissolve the residue in 200 μl ethyl acetate


Step 2:
Column conditioning:
1 ml hexane

Sample application:
Slowly force or aspirate the final solution from step 1 through the column

Column washing:
ethyl acetate

Elution:
1 ml acetone / hexane (9:1, v/v), then 1 ml acetone
Dry eluate in a stream of nitrogen, wash the residue twice with hexane and
redissolve the remaining residue, which is insoluble in hexane, in di-2-propyl
ether. Evaporate the ether fraction to dryness and redissolve in 100 μl ethyl
acetate. These last purification steps allow further discrimination of
interfering sewage water components.
Part of the final ethyl acetate fraction was derivatised with trifluoroacetic
anhydride at 80 °C for 20 min.
Authors: Steger-Hartmann T Kümmerer K Schecker J
Source: J Chromatogr 726 (1996) 179 - 184


Details


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