Burcu Sen-Utsukarci, Turgut Taskin, Fatih Goger, Nurhayat Tabanca, Alden S. Estep, Sonja M. Kessler, Ozlem Akbal-Dagistan, Hilal Bardakci, Mine Kurkcuoglu, James Becnel, Alexandra Kiemer, Afife Mat, Burcu Sen-Utsukarci, Turgut Taskin, Fatih Goger, Nurhayat Tabanca, Alden S. Estep, Sonja M. Kessler, Ozlem Akbal-Dagistan, Hilal Bardakci, Mine Kurkcuoglu, James Becnel, Alexandra Kiemer, and Afife Mat
Valeriana is a common plant species used for various healing purposes in folk medicine since antiquity. This study investigates the phytochemical profile, antioxidant, cytotoxic, and insecticidal activity of Valeriana alliariifolia Adams, a species that has traditionally been used in Turkey. For the analyses we prepared four root extracts of V. alliariifolia Adams using hexane (HM1), chloroform (CM1), ethanol (EM1), and water (WM1) for maceration. Additionally, two extracts were also prepared from its roots by maceration separately with ethanol (EM2) and water (WM2). One sample was prepared as a water infusion (WI), according to the procedure used in Turkish traditional medicine. The 2,2-Diphenyl-1-picrylhydrazyl (DPPH) scavenging and 2,2’-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid (ABTS) radical cation scavenging activity tests showed that ethanol extracts had the strongest antioxidant activity: EM1 (IC50 – DPPH: 17.694 μg/mL; ABTS: 23.8 μg/mL) and EM2 (IC50 – DPPH: 20 μg/mL; ABTS: 21.5 μg/mL). The hexane extract, HM1, was the most cytotoxic (IC50<10 μg/mL against HepG2 and HUVEC) and EM2 strongly cytotoxic (IC50<10 μg/mL against HepG2 and IC50: 11.96 μg/mL against HUVEC). The extracts with demonstrated cytotoxic activities were further examined to check their insecticidal activity against adult female mosquito Aedes aegypti and first instar Ae. aegypti larvae. HM1 was the most effective (90±10 %), which was consistent with its cytotoxic activity. Because of the high antioxidant, cytotoxic, and insecticidal activities, we ran phytochemical analyses of the HM1, EM1, and EM2 extracts with GC-MS (for HM1) and LC-MS/MS (for EM1 and EM2). We also analysed the composition of the essential oil obtained from V. alliariifolia roots by micro-distillation in order to compare its content with HM1, which contains volatile compounds. Phytochemical analyses revealed that the major compound in HM1 was isovaleric acid (16 %) and in the essential oil 1,8-cineole (2.9 %). EM1, Valerijana (odoljen) česta je biljna vrsta koja se zbog svojih ljekovitih svojstava od davnina rabi u narodnoj medicini. U ovome se istraživanju utvrdio fitokemijski profil te antioksidacijsko, citotoksično i insekticidno djelovanje tradicionalne vrste koja se za liječenje rabi u Turskoj – Valeriana alliariifolia Adams. Za analizu je maceracijom pripremljeno šest ekstrakata njezina korijena pomoću heksana (HM1), kloroforma (CM1), etanola (EM1, EM2) i vode (WM1, WM2). Jedan je uzorak pripremljen infuzijom vodom (WI) prema tradicionalnom turskom receptu za ljekovite pripravke. Testovima antioksidacijskoga djelovanja pomoću 2,2-difenil-1-pikrilhidrazila (DPPH) i 2,2’-azino-bis(3-etilbenzotiazolin-6-sulfonične kiseline (ABTS) izdvojeni su sljedeći ekstrakti s najjačim antioksidacijskim djelovanjem: EM1 (IC50 – DPPH: 17,694 μg/mL; ABTS: 23,8 μg/mL) i EM2 (IC50 – DPPH: 20 μg/mL; ABTS: 21,5 μg/mL). Ekstrakt s heksanom, HM1, iskazao je najveću citotoksičnost (IC50<10 μg/mL protiv tumorskih stanica HepG2 i HUVEC), a EM2 snažnu citotoksičnost (IC50<10 μg/mL protiv HepG2 stanica te IC50 11,96 μg/mL protiv HUVEC stanica). Ekstrakte s najsnažnijim citotoksičnim djelovanjem također smo analizirali za insekticidno djelovanje protiv odraslih ženki komarca vrste Aedes aegypti te njihovih ličinki. U skladu sa svojom citotoksičnosti, HM1 se pokazao najdjelotvornijim (smrtnost 90±10 %). Zbog snažnog antioksidacijskog, citotoksičnog i insekticidnog djelovanja, napravili smo i fitokemijsku analizu ekstrakata HM1, EM1 i EM2 služeći se metodama GC-MS (za HM1) i LC-MS/MS (za EM1 i EM2). Također smo analizirali sastav esencijalnoga ulja dobivenoga mikrodestilacijom korijena V. alliariifolia kako bismo ga usporedili sa sastavom HM1, koji je sadržavao hlapljive sastojke. Fitokemijska je analiza pokazala da je glavni sastojak HM1 izovalerijanska kiselina (16 %), a esencijalnoga ulja 1,8-cineol (2,9 %). Glavni sastojci ekstrakata EM1 i EM2 bili su 5-O-kafeoilkvinska kiselina (klorogena kiselina)