Headspace Solid Phase Microextraction for Terpenes and Volatile Compounds Determination in Mastic Gum Extracts, Mastic Oil and Human Urine by GC– MS

Abstract

A reliable analytical method was developed, which is based on Headspace Solid Phase Microextraction (HS-SPME) and Gas Chromatography–Mass Spectrometry (GC-MS) for the detection of volatile components of the gum and the essential oil of Pistacia lentiscus var. chia, commonly known as mastic gum and mastic oil respectively. The conditions of the HS-SPME were optimized and aqueous-ethanolic extracts of mastic gum and solutions of mastic oil in ethanol-water were analyzed by GC-MS. Almost 26 volatile components in mastic gum and 34 in mastic oil were identified in the gum and the oil respectively. The major constituents of the mastic gum and the mastic oil were α-pinene (63% and 76%, respectively), β-myrcene (15% and 14%), β-pinene (4% and 4%), limonene (2.5% and 1.5%), and caryophyllene (5% and 1%). The quantitative determination of six of the aforementioned substances in multi-analyte standard solutions was achieved with good performance features. The repeatability (RSD%) was <4.2% and the limits of detection were 1.2 µg/L for α-pinene, 0.09 µg/L for β-pinene, 0.7 µg/L for β-myrcene, 0.02 µg/L for camphene, 0.02 µg/L for p-cymene, and 0.07 µg/L for α-terpineol. The HS-SPME/GC-MS procedure was successfully applied to samples of human urine samples after dietetic use of various mastic products such as mastic gum, mastic oil and Greek traditional highly viscous white mastic sweet. Traces of several constituents of mastic, such as α-pinene, β-myrcene, limonene, p-methyl anisole, terpinene, carveol, myrtenol, caryophyllene, α-caryophyllene, and so forth, were detected in the collected urine samples.