Headspace solid-phase microextraction gas chromatography-mass spectrometry analysis of volatiles in orujo spirits from a defined geographical origin.
A headspace solid-phase microextraction (HS-SPME) and gas chromatography-selective ion monitoring/mass spectrometry (GC-SIM/MS) method was optimized for analysis of 22 volatile compounds in orujo spirit samples from the Geographic Denomination "Orujo de Galicia/Augardente de Galicia". HS-SPME experimental conditions, such as fiber coating, extraction temperature, extraction and pre-equilibrium time, sample volume, and the presence of salt, were studied to improve the extraction process. The best results were obtained using a 65 microm Carbowax-divinylbenzene fiber during a headspace extraction at 40 degrees C with constant magnetic stirring for 15 min and after a 5 min period of pre-equilibrium time. The sample volume was 6 mL of orujo containing 25% of NaCl, placed in 12 mL glass vials equipped with a screw cap and PTFE/silicone septum. Desorption was performed directly in the gas chromatograph injector port for 5 min at 250 degrees C using the splitless mode. The proposed method is sensible (with detection limits between 0.0045 and 0.2399 mg/L), precise (with coefficients of variation in the range 0.99-8.18%), and linear over more than 1 order of magnitude. The developed method presented recoveries comprised between 76.0 and 112.4%. The applicability of the new method was demonstrated by determining the considered 22 volatile compounds in nine orujo commercial samples with quality and origin brands.
Peña
Rosa M
RM
Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias, Universidad de Santiago de Compostela, Avda. Alfonso X El Sabio s/n, 27002 Lugo, Spain.
Barciela
Julia
J
Herrero
Carlos
C
García-Martín
Sagrario
S
D000434:Alcoholic Beverages / Q000032:analysis*; D000438:Alcohols / Q000032:analysis; D005232:Fatty Acids, Volatile / Q000032:analysis; D005638:Fruit; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D009812:Odorants / Q000032:analysis; D012680:Sensitivity and Specificity; D013729:Terpenes / Q000032:analysis; D027843:Vitis; D014835:Volatilization
D000438:Alcohols; D005232:Fatty Acids, Volatile; D013729:Terpenes