Pregled ponudbe izbranih hidrolatov na slovenskem trgu in analiza sestave hidrolata laškega smilja (Helichrysum italicum)

Štumberger, Rok (author), Kočevar Glavač, Nina (mentor), Kokalj Ladan, Meta (co-mentor)

V magistrski nalogi smo proučevali kvalitativno in kvantitativno sestavo hidrolatov laškega smilja (Helychrisum italicum) z metodo plinske kromatografije, sklopljene z masno spektroskopijo (GC-MS). Naredili smo tudi pregled ponudbe hidrolatov na slovenskem trgu. Ugotovili smo, da so hidrolati na slovenskem trgu razširjeni. Največja ponudba je na spletnih straneh, nekaj je lokalnih pridelovalcev, nekateri hidrolati pa so dostopni tudi v večjih trgovinah. Med najpogostejšimi hidrolati so hidrolati sivke, laškega smilja, rožmarina in damaščanske vrtnice. Analizirali smo sestavo 12-tih hidrolatov laškega smilja različnih proizvajalcev. V okviru optimizacije metode ekstrakcije glede občutljivosti, ponovljivosti metod in izkoristka ekstrakcije smo za nadaljnjo analizo vzorcev izbrali metodo dvojne ekstrakcije s heksanom v razmerju 1 : 1 (V/V) in injiciranje z linearno delitvijo vzorca (»split«) 1 : 10. Pri neposredni analizi neobdelanih hidrolatov laškega smilja smo identificirali med 11 in 38 različnih spojin, v 1. ekstraktih hidrolatov med 19 in 58, v 2. ekstraktih pa med 4 in 22 spojin. Največji delež (> 1%) identificiranih spojin v 1. ekstraktih so predstavljale spojine, ki spadajo v skupino alkoholnih monoterpenoidov (α-terpineol, linalool, nerol, evkaliptol in borneol), ketonov (4-6-dimetiloktan-3,5-dion, pentan-3-on, izopropil-etilketon, 4,6,9-trimetil-8-decen-3,5-dion (»italadion«)) in n-undekan, ki spada med oglikovodike. Med posameznimi spojinami je v 1. ekstraktih prevladoval α-terpineol s povprečno vsebnostjo (20,1 %), sledili pa so mu 4,6-dimetiloktan-3,5-dion (11,2 %), linalool (7,5 %) in pentan-3on (6,9 %). V 2. ekstraktih je prevladoval pentan-3-on. Pri neposredni analizi neobdelanih hidrolatov smo identificirali nekaj spojin, ki se v ekstraktih niso pojavljale. Med njimi so bile razne kisline (fosfonska kislina, etanojska kislina, karbaminska kislina, benzojska kislina) in soli (sol benzojske kisline, sol karbaminske kisline). Za izbranih šest spojin (α-terpineol, linalool, pentan-3-on, evkaliptol, nerol in borneol) smo ocenili ponovljivost meritev in jih kvantificirali z uporabo eksternih standardov. Koncentracije izbranih 6-ih spojin bile med 30 in 395 mg/L. Primerjali smo tudi koncentracije celokupnih hlapnih spojin, ki smo jih preračunali iz relativnih deležev izbranih šestih spojin in njihovih koncentracij. Celokupne koncentracije hlapnih spojin, v izbranih hidrolatih, so bile med 800 mg/L in 100 mg/L. Ugotovili smo, da se hidrolati laškega smilja med seboj zelo razlikujejo po številu, koncentraciji in relativnem deležu spojin, so pa si med seboj podobni po spojinah, ki prevladujejo.

• Language: Slovenian
• Keywords: GC-MS, Helychrisum italicum, hidrolat, sestava
• Work type: Master's thesis/paper
• Organization: FFA - Faculty of Pharmacy
• Year: 2023
• PID: 20.500.12556/RUL-145782
• Publication date in RUL: 14.05.2023

Secondary language

• Language: English
• Title: Market analysis of selected hydrolates on Slovenian market and chemical composition analysis of Helichrysum italicum hydrolate

Abstract

In the Master's thesis we studied qualitative and quantitative composition of hydrosols using gas chromatography coupled with mass spectroscopy (GC-MS). We also made a review of hydrolates that are avaliable on Slovenian market. They are mainly available in online shops, while minor supply is through local producers and larger stores. Most frequent were hydrosols of Lavandula angustifolia, Helychrisum italicum, Rosmarinus officinalis and Rosa damascena. We analyzed the compostion of 12 Helychrisum italicum hydrosols of various manufacturers. After evaluating the sensitivity, repeatability and extraction yield, we chose double extraction with hexane(1:1 V/V ratio) and split ratio 1:10. In direct hydrolate analysis, we identified 11–38 different compounds, in 1. extracts 19–58 compunds, while in 2. extracts there were 4–22 compounds. Compounds that were in higher contents (>1% of total volatiles) in 1. extracts were alcoholic monoterpenoids (α-terpineol, linalool, nerol, eucalyptol and borneol), ketones (4-6-dimethyloctan-3,5-dione, pentan-3-one, izopropil-etilketon, 4,6,9-trimethyl-8-decene-3,5-dione (»italadion«)) and n-undecane, an alkane. On average, terpineol-α represented the highest percentage of overall composition (20,10%) followed by 4,6-dimethyloctan-3,5-dione (11,24%), linalool (7,52%) and pentan-3one (6,87%). On average, pentan-3-one represented the highest percentage of compounds in 2. extracts. Some of compunds found in direct hydrolate analysis were detected only in direct samples and not in extracts. Those were various acids (phosphonic acid, etanoic acid, carbamic acid, benzoic acid) and salts (benzoic acid salt, carbamic acid salt). We chose 6 compounds (α-terpineol, linalool, pentan-3-one, eucalyptol, nerol and borneol) and quantified them using the external standard method and evaluated repeatability of measurements. Average concetrations of all 6 compounds were 30–395 mg/L. We also calculated total concentration of volatiles by using concentrations of 6 chosen compounds and their percentage of total volatiles. Total concentration of volatiles, in chosen hydrolates, ranged from 800 mg/L to 100 mg/L. We concluded that hydrosols of Helychrisum italicum differ in the number, relative proportion and concentration of volatile compounds. However compounds that represent most of the composition are similar.

• Keywords: GC-MS, Helychrisum italicum, hydrolate, hydrosol, composition