Analiza hidrolatov navadnega lovorja (Laurus nobilis), grenkega pomarančevca (Citrus × aurantium) in damaščanske vrtnice (Rosa × damascena) s slovenskega tržišča

Ukmar, Matis (author), Kočevar Glavač, Nina (mentor), Schoss, Katja (comentor)

Magistrska naloga se osredotoča na analizo hidrolatov treh rastlin, in sicer petih hidrolatov navadnega lovorja (Laurus nobilis), sedmih hidrolatov grenkega pomarančevca (Citrus × aurantium) in devetih hidrolatov damaščanske vrtnice (Rosa × damascena), ki so prisotni na slovenskem tržišču. Glavni cilj naloge je preučiti sestavo hidrolatov s pomočjo plinske kromatografije, sklopljene z masno spektrometrijo (GC-MS). Hidrolate smo analizirali z neposredno analizo hidrolatov ter z analizo izvlečkov, pridobljenih s heksanom in etilacetatom. V okviru analiz smo določili glavne spojine v hidrolatih posameznih rastlin. Glavne spojine so tiste, ki predstavljajo največje relativne površine vrhov (A [%]). Pri hidrolatu navadnega lovorja so to bile naslednje spojine: evkaliptol, linalol, α-terpineol, terpinen-4-ol, metilevgenol, evgenol in elemicin. Pri hidrolatu damaščanske vrtnice so to bile: citronelol, geraniol, nerol, linalol, α-terpineol, terpinen-4-ol, 2-feniletanol, metilevgenol in evgenol. V hidrolatu grenkega pomarančevca pa so to bile: linalol, α-terpineol, terpinen-4-ol, nerol, geraniol, metilantranilat, benzil nitril ter cis- in trans-linalol oksid. Poleg tega smo izvedli tudi kvantitativno analizo dišavnih alergenov in metilevgenola ter preverili skladnost hidrolatov z zahtevami evropske Uredbe o kozmetičnih izdelkih (ES št.: 1223/2009). Ugotovili smo, da pri kar 38 % (8 od 21) analiziranih hidrolatov dišavni alergeni niso bili ustrezno navedeni. Metilevgenol je presegal koncentracijsko mejo 2 mg/L pri 62 % (13 od 21) izdelkov, in sicer pri petih hidrolatih navadnega lovorja in pri osmih hidrolatih damaščanske vrtnice. V celoti je le 24 % (5 od 21) hidrolatov ustrezalo vsem zahtevam Uredbe o kozmetičnih izdelkih. V okviru ovrednotenja sestave smo izvedli še primerjavo med neposredno analizo hidrolata ter analizo heksanskih in etilacetatnih izvlečkov hidrolatov. Med etilacetatnimi in heksanskimi izvlečki ni bilo statistično značilne razlike glede občutljivosti, saj sta obe metodi zaznali primerljivo število spojin in dišavnih alergenov. Pomanjkljivost analize etilacetatnih izvlečkov pa je bila slabša ponovljivost. Metodi etilacetatne ekstrakcije in neposredne analize hidrolata sta bili bolj občutljivi pri detekciji bolj polarnih spojin. To smo opazili pri zaznavi oksidov linalola in cis-terpin hidratu. Uporaba metode neposredne analize hidrolata je precej zanimiva s stališča hitre kvalitativne in kvantitativne analize najbolj zastopanih spojin, saj je nezahtevna, časovno najkrajša in najboljše prikaže realno sestavo hidrolatov.

• Language: Slovenian
• Keywords: analiza GC-MS, dišavni alergeni, evropska Uredba o kozmetičnih izdelkih, hidrolati, metilevgenol.
• Work type: Master's thesis/paper
• Organization: FFA - Faculty of Pharmacy
• Year: 2025
• PID: 20.500.12556/RUL-173720
• Publication date in RUL: 20.09.2025

Secondary language

• Language: English
• Title: Analysis of bay laurel (Laurus nobilis), bitter orange (Citrus × aurantium) and Damask rose (Rosa × damascena) hydrolates from the Slovenian market

Abstract

The master's thesis focuses on the analysis of hydrolates from three plant species, namely five hydrolates of bay laurel (Laurus nobilis), seven hydrolates of bitter orange (Citrus × aurantium), and nine hydrolates of Damask rose (Rosa × damascena) available on the Slovenian market. The main objective of this work was to study the composition of hydrolates using gas chromatography coupled with mass spectrometry (GC-MS). The hydrolates were analyzed both directly and through extracts obtained using hexane and ethyl acetate. During the analyses, the compounds with the largest relative area of peaks present in each plant hydrolates were identified. In bay laurel hydrolates, these compounds were eucalyptol, linalool, α-terpineol, terpinen-4-ol, methyl eugenol, eugenol, and elemicin. In Damask rose hydrolates, these compounds were citronellol, geraniol, nerol, linalool, α-terpineol, terpinen-4-ol, 2-phenylethanol, methyl eugenol, and eugenol. In bitter orange hydrolates, these compounds were linalool, α-terpineol, terpinen-4-ol, nerol, geraniol, methyl anthranilate, benzil nitrile, and cis- and trans-linalool oxide. In addition, a quantitative analysis of fragrance allergens and methyl eugenol was carried out, and the compliance of the hydrolates with the European Cosmetics Regulation (EC No 1223/2009) was assessed. The results showed that 38% (8 of 21) of the analyzed hydrolates failed to properly declare fragrance allergens. Furthermore, methyl eugenol concentrations exceeded the 2 mg/L limit in 62% (13 of 21) hydrolates, specifically in five bay laurel hydrolates and eight Damask rose hydrolates. Overall, only 24% (5 of 21) hydrolates complied with all requirements of the cosmetics regulation. Finally, a comparison was made between the direct hydrolate analysis and the analysis of hydrolate extracts obtained with hexane and ethyl acetate. No statistically significant difference in sensitivity was observed between the ethyl acetate and hexane extracts, as both methods detected a comparable number of compounds and fragrance allergens. However, a drawback of ethyl acetate extraction was its poorer repeatability. Both ethyl acetate extraction and direct hydrolate analysis proved to be more sensitive in detecting more polar compounds, as observed in the detection of linalool oxides and cis-terpine hydrate. The use of direct hydrolate analysis is interesting for rapid qualitative and quantitative analysis of the most abundant compounds, as it is simple, time-efficient, and provides a realistic picture of the hydrolate composition.

• Keywords: European Cosmetics Regulation, fragrance allergens, GC-MS analysis, hydrolates, methyl eugenol.