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Herbs and spices: characterization and quantitation of biologically-active markers for routine quality control by multiple headspace solid-phase microextraction combined with separative or non-separative analysis.

Journal of chromatography. A (2014-12-30)
Barbara Sgorbini, Carlo Bicchi, Cecilia Cagliero, Chiara Cordero, Erica Liberto, Patrizia Rubiolo
ABSTRACT

Herbs and spices are used worldwide as food flavoring, thus determination of their identity, origin, and quality is mandatory for safe human consumption. An analysis strategy based on separative (HS-SPME-GC-MS) and non-separative (HS-SPME-MS) approaches is proposed for the volatile fraction of herbs and spices, for quality control and to quantify the aromatic markers with a single analysis directly on the plant material as such. Eight-to-ten lots of each of the following herbs/spices were considered: cloves (Syzygium aromaticum (L.) Merr. & Perry), American peppertree (Schinus molle L.), black pepper and white pepper (Piper nigrum L.), rosemary (Rosmarinus officinalis L.), sage (Salvia officinalis L.) and thyme (Thymus vulgaris L.). Homogeneity, origin, and chemotypes of the investigated lots of each herb/spice were defined by fingerprinting, through statistical elaboration with principal component analysis (PCA). Characterizing aromatic markers were directly quantified on the solid matrix through multiple headspace extraction-HS-SPME (MHS-SPME). Reliable results were obtained with both separative and non-separative methods (where the latter were applicable); the two were in full agreement, RSD% ranging from 1.8 to 7.7% for eugenol in cloves, 2.2-18.4% for carvacrol+thymol in thyme, and 3.1-16.8% for thujones in sage.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Thymol, ≥98.5%
Sigma-Aldrich
Divinylbenzene, technical grade, 80%
Sigma-Aldrich
Eugenol, ReagentPlus®, 99%
Sigma-Aldrich
Linalool, 97%
Sigma-Aldrich
Terpineol, mixture of isomers, anhydrous
Sigma-Aldrich
Thymol, meets analytical specification of Ph. Eur., BP, NF, 99-101%
Sigma-Aldrich
Eugenol, natural, ≥98%, FG
Supelco
Linalool, analytical standard
Sigma-Aldrich
Linalool, ≥97%, FCC, FG
Sigma-Aldrich
Thymol, FCC, FG
Supelco
Thymol, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Divinylbenzene, technical grade, 55%
Sigma-Aldrich
Dipentene, technical, for use as solvent (for the paint industry), mixture of various terpenes
Sigma-Aldrich
Eugenol, ≥98%, FCC, FG
Sigma-Aldrich
(−)-Bornyl acetate, 95%
Supelco
Eugenol, PESTANAL®, analytical standard
Supelco
Eugenol, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Thymol, analytical standard
Sigma-Aldrich
(−)-Linalool, ≥95.0% (sum of enantiomers, GC)
Sigma-Aldrich
Poly(dimethylsiloxane), viscosity 1.0 cSt (25 °C)
Supelco
(−)-Bornyl acetate, analytical standard
Supelco
Eugenol, certified reference material, TraceCERT®
Supelco
(−)-Linalool, analytical standard
Sigma-Aldrich
Hexamethyldisiloxane, viscosity 0.65 cSt (25 °C)
Supelco
Thymol, Standard for quantitative NMR, TraceCERT®
Sigma-Aldrich
Dipentene, mixture of isomers
Supelco
Terpineol, mixture of isomers, analytical standard
Supelco
SPME Portable Field Sampler, coating PDMS
Supelco
SPME/HPLC Interface, rheodyne valve version
Supelco
SPME Sampling Stand, for use with 15 mL vials