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Headspace solid-phase microextraction-gas chromatography-mass spectrometry characterization of propolis volatile compounds.
J Pharm Biomed Anal. 2013 Oct; 84:103-11.JP

Abstract

In this study, a novel and efficient method based on headspace solid-phase microextraction (HS-SPME), followed by gas chromatography-mass spectrometry (GC-MS), was developed for the analysis of propolis volatile compounds. The HS-SPME procedure, whose experimental parameters were properly optimized, was carried out using a 100 μm polydimethylsiloxane (PDMS) fiber. The GC-MS analyses were performed on a HP-5 MS cross-linked 5% diphenyl-95% dimethyl polysiloxane capillary column (30 m × 0.25 mm I.D., 1.00 μm film thickness), under programmed-temperature elution. Ninety-nine constituents were identified using this technique in the samples of raw propolis collected from different Italian regions. The main compounds detected include benzoic acid (0.87-30.13%) and its esters, such as benzyl benzoate (0.16-13.05%), benzyl salicylate (0.34-1.90%) and benzyl cinnamate (0.34-3.20%). Vanillin was detected in most of the samples analyzed in this study (0.07-5.44%). Another relevant class of volatile constituents is represented by sesquiterpene hydrocarbons, such as δ-cadinene (1.29-13.31%), γ-cadinene (1.36-8.85%) and α-muurolene (0.78-6.59%), and oxygenated sesquiterpenes, such as β-eudesmol (2.33-12.83%), T-cadinol (2.73-9.95%) and α-cadinol (4.84-9.74%). Regarding monoterpene hydrocarbons, they were found to be present at low level in the samples analyzed in this study, with the exception of one sample from Southern Italy, where α-pinene was the most abundant constituent (13.19%). The results obtained by HS-SPME-GC-MS were also compared with those of hydrodistillation (HD) coupled with GC-MS. The HS-SPME-GC-MS method developed in this study allowed us to determine the chemical fingerprint of propolis volatile constituents, thus providing a new and reliable tool for the complete characterization of this biologically active apiary product.

Authors+Show Affiliations

Department of Life Sciences, University of Modena and Reggio Emilia, Via G. Campi 183, 41125 Modena, Italy. federica.pellati@unimore.itNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

23807002

Citation

Pellati, Federica, et al. "Headspace Solid-phase Microextraction-gas Chromatography-mass Spectrometry Characterization of Propolis Volatile Compounds." Journal of Pharmaceutical and Biomedical Analysis, vol. 84, 2013, pp. 103-11.
Pellati F, Prencipe FP, Benvenuti S. Headspace solid-phase microextraction-gas chromatography-mass spectrometry characterization of propolis volatile compounds. J Pharm Biomed Anal. 2013;84:103-11.
Pellati, F., Prencipe, F. P., & Benvenuti, S. (2013). Headspace solid-phase microextraction-gas chromatography-mass spectrometry characterization of propolis volatile compounds. Journal of Pharmaceutical and Biomedical Analysis, 84, 103-11. https://doi.org/10.1016/j.jpba.2013.05.045
Pellati F, Prencipe FP, Benvenuti S. Headspace Solid-phase Microextraction-gas Chromatography-mass Spectrometry Characterization of Propolis Volatile Compounds. J Pharm Biomed Anal. 2013;84:103-11. PubMed PMID: 23807002.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Headspace solid-phase microextraction-gas chromatography-mass spectrometry characterization of propolis volatile compounds. AU - Pellati,Federica, AU - Prencipe,Francesco Pio, AU - Benvenuti,Stefania, Y1 - 2013/06/03/ PY - 2013/03/13/received PY - 2013/05/24/revised PY - 2013/05/27/accepted PY - 2013/6/29/entrez PY - 2013/6/29/pubmed PY - 2014/2/28/medline KW - DVB-CAR-PDMS KW - Gas chromatography KW - HD KW - HS KW - LRI KW - Mass spectrometry KW - PDMS KW - Propolis KW - Solid-phase microextraction KW - Volatile compounds KW - divinylbenzene-carboxen-polydimethylsiloxane KW - headspace KW - hydrodistillation KW - linear retention index KW - polydimethylsiloxane SP - 103 EP - 11 JF - Journal of pharmaceutical and biomedical analysis JO - J Pharm Biomed Anal VL - 84 N2 - In this study, a novel and efficient method based on headspace solid-phase microextraction (HS-SPME), followed by gas chromatography-mass spectrometry (GC-MS), was developed for the analysis of propolis volatile compounds. The HS-SPME procedure, whose experimental parameters were properly optimized, was carried out using a 100 μm polydimethylsiloxane (PDMS) fiber. The GC-MS analyses were performed on a HP-5 MS cross-linked 5% diphenyl-95% dimethyl polysiloxane capillary column (30 m × 0.25 mm I.D., 1.00 μm film thickness), under programmed-temperature elution. Ninety-nine constituents were identified using this technique in the samples of raw propolis collected from different Italian regions. The main compounds detected include benzoic acid (0.87-30.13%) and its esters, such as benzyl benzoate (0.16-13.05%), benzyl salicylate (0.34-1.90%) and benzyl cinnamate (0.34-3.20%). Vanillin was detected in most of the samples analyzed in this study (0.07-5.44%). Another relevant class of volatile constituents is represented by sesquiterpene hydrocarbons, such as δ-cadinene (1.29-13.31%), γ-cadinene (1.36-8.85%) and α-muurolene (0.78-6.59%), and oxygenated sesquiterpenes, such as β-eudesmol (2.33-12.83%), T-cadinol (2.73-9.95%) and α-cadinol (4.84-9.74%). Regarding monoterpene hydrocarbons, they were found to be present at low level in the samples analyzed in this study, with the exception of one sample from Southern Italy, where α-pinene was the most abundant constituent (13.19%). The results obtained by HS-SPME-GC-MS were also compared with those of hydrodistillation (HD) coupled with GC-MS. The HS-SPME-GC-MS method developed in this study allowed us to determine the chemical fingerprint of propolis volatile constituents, thus providing a new and reliable tool for the complete characterization of this biologically active apiary product. SN - 1873-264X UR - https://www.unboundmedicine.com/medline/citation/23807002/Headspace_solid_phase_microextraction_gas_chromatography_mass_spectrometry_characterization_of_propolis_volatile_compounds_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0731-7085(13)00246-X DB - PRIME DP - Unbound Medicine ER -