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  • Solid-phase microextraction (SPME) analysis of six Italian populations of Ephedra nebrodensis Tineo ex Guss. subsp. nebrodensis.

Solid-phase microextraction (SPME) analysis of six Italian populations of Ephedra nebrodensis Tineo ex Guss. subsp. nebrodensis.

Chemistry & biodiversity (2011-01-25)
Filippo Maggi, Marcello Nicoletti, Valentina Petitto, Gianni Sagratini, Fabrizio Papa, Sauro Vittori
RESUMEN

Headspace solid-phase microextraction (HS-SPME) coupled with GC/FID and GC/MS was applied for the first time in the analysis of the volatile fraction of an Ephedra species. Notably, six Italian populations (Marche, Abruzzo, and Sardinia) of Ephedra nebrodensis subsp. nebrodensis, covering almost the entire Italian area, were investigated to examine the chemical variability and to support the taxonomy of the species. A fiber screening with polymethylsiloxane (PDMS), Carboxen(TM) /polymethylsiloxane (CAR/PDMS), and polymethylsiloxane/divinylbenzene (PDMS/DVB) coatings, together with an optimization of the extraction conditions were carried out before analysis of the six populations. A total of 119 volatiles were identified in the headspace of different samples, accounting for 63.35-100.00% of the total volatiles. A great variability was found in the qualitative composition of different samples, since only 18 components were in common among all populations. The headspace composition was dominated by sesquiterpene hydrocarbons (52.30-88.32%), with β-maaliene (traces-7.49%), β-patchoulene (traces-1.29%), β-panasinsene (traces-6.85%), α-isocomene (traces-31.25%), α-trans-bergamotene (traces-6.95%), alloaromadendrene (traces-33.20%), α-acoradiene (traces-9.41%), and γ-muurolene (0.61-16.33%) being the most abundant constituents. Noteworthy is the occurrence in a sample of two major unknown sesquiterpenes, one hydrocarbon (24.49%, RI: 1396) and one oxygenated compound (10.37%, RI: 1591), whose mass spectra were reported for the first time. Multivariate chemometric techniques, such as cluster analysis (CA) and principal component analysis (PCA), were used to characterize the samples according to the geographical origin.

MATERIALES
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Supelco
Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, needle size 24 ga, StableFlex
Supelco
Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, needle size 24 ga, for use with manual holder
Supelco
Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, needle size 23 ga, StableFlex, for use with autosampler
Supelco
Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, needle size 23 ga, StableFlex, for use with manual holder or autosampler, fiber L 2 cm
Supelco
Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, needle size 24 ga, StableFlex, for use with autosampler
Supelco
ORBO 90 Carboxen® 564 (20/45) 160/80 mg, W,F,F separators, O.D. × L 6 mm × 75 mm, pkg of 25 ea, for analyte group MEK (methylethyl ketone)
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ORBO-78 400/200 MG PK/25, W,W,W separators, O.D. × L 6 mm × 110 mm, pkg of 25 ea
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Carboxen® Adsorbent, matrix Carboxen® 1000, 60-80 mesh, bottle of 10 g
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Columna capilar para GC Carboxen®-1010 PLOT, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
Supelco
Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 75 μm(CAR/PDMS, for use with manual holder, needle size 24 ga
Supelco
Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 85 μm(CAR/PDMS, needle size 23 ga, StableFlex, for use with autosampler
Supelco
Columna capilar para GC Carboxen®-1006 PLOT, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
Supelco
Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 75 μm(CAR/PDMS, needle size 24 ga, for use with autosampler
Supelco
Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 85 μm(CAR/PDMS, needle size 24 ga, StableFlex, for use with autosampler
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Columna capilar para GC Carboxen®-1010 PLOT, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
Supelco
Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 85 μm(CAR/PDMS, needle size 24 ga, for use with manual holder, StableFlex fiber
Supelco
Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 75 μm(CAR/PDMS, needle size 23 ga, for use with autosampler
Supelco
Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 75 μm(CAR/PDMS, needle size 23 ga, for use with manual holder
Supelco
Carboxen® Adsorbent, matrix Carboxen® 572, 20-45 mesh, bottle of 10 g
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Columna capilar para GC Carboxen®-1006 PLOT, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
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Tenax® TA / Carboxen® 1018, glass TD tube, preconditioned, O.D. × L 1/4 in. × 3 1/2 in., Sealed with (Swagelok® End-Fittings), pkg of 10 ea
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Carboxen® Adsorbent, matrix Carboxen® 1000, 40-60 mesh, bottle of 50 g
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Carboxen® Adsorbent, matrix Carboxen® 569, 20-45 mesh, bottle of 10 g
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Carboxen® Adsorbent, matrix Carboxen® 1003, 40-60 mesh, bottle of 10 g
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Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 2 cm
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Carboxen® 1000 Reversible SPE Tube, 200 mg/mL, pk 30
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Tubo absorbente ORBO-93, ORBO tube I.D. × L 6 mm × 95 mm, Bed A 180 mg, Bed B 90 mg, 60/80 mesh, pkg of 25 ea
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Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 1 cm
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Carboxen® Adsorbent, matrix Carboxen® 569, 20-45 mesh, bottle of 500 g
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Carboxen® Adsorbent, matrix Carboxen® 563, 20-45 mesh, bottle of 10 g