Chemicals. HPLC grade solvents and water purified by
deionization and 0.22-ím membrane filtration (Millipore) were
used. Methanol-d4 (99.8 atom % deuterium) was obtained from
Armar Chemicals (Do¨ttingen, Switzerland). Pure, authentic thapsigargin
(1) and compound 6 were available from previous studies.
Sample Preparation. Fruits of T. garganica L. (Apiaceae)
were collected on Ibiza, Spain, in July 2002; a voucher specimen
(DFHSBC1) was deposited in Herbarium C (Botanical Museum,
University of Copenhagen, Denmark). The powdered fruits (20
g) were extracted with 200 mL of 96% ethanol at ambient
temperature for 6 h. Half of the extract was evaporated in vacuo
and partitioned between water and toluene; evaporation of the
toluene phase gave 374 mg of the extract, dissolved in acetonitrile
(31 mg/mL) for HPLC-SPE analysis. Authentic thapsigargin (1)
in acetonitrile (48 mg/mL) and 6 (2 mg/mL) were used as
standards.