TY  - CONF
AU  - Mutavski, Zorana
AU  - Ćujić-Nikolić, Nada
AU  - Radan, Milica
AU  - Bigović, Dubravka
AU  - Marković, Smilja
AU  - Šavikin, Katarina
PY  - 2022
UR  - https://dais.sanu.ac.rs/123456789/13503
AB  - Everlasting flowers (Helichrysum plicatum L.), traditionally used for gastrointestinal disorders such as abdominal pain, jaundice, and hepatic disorders are a rich source of sensitive polyphenolic compounds whose preservation is of great importance. A critical point in the development of formulations with bioactive phenolic compounds, especially liquid extracts is their limited stability at elevated temperatures, pH variations, exposure to oxygen, light, and moisture. In order to overcome the extract limitations, drying method could be the optimal technique for preservation of bioactive compounds, in order to obtain stable powders with appropriate characteristics. One of the most advanced techniques based on the phenomenon of sublimation is a freeze drying, which enabling the long-term preservation of heat-sensitive compounds. In this study, extract obtained by percolation method was lyophilized by freeze drying method (firstly extract was frozen at -80 oC for 1 h, then freeze- dried at -60 oC with pressure of 0.011 mbar for 24 h, and finally main dried at -60 oC with pressure of 0.0012 mbar, for an additional hour in order to remove the capillary water residues). The obtained freeze-dried extract (FHE) was characterized by drying efficiency, the contents of total polyphenols-TPC and flavonoids-TFC. The most dominant polyphenolic compounds were determined and quantified by HPLC method. Differential scanning calorimetry (DSC) and scanning electron microscopy (SEM) analyzes were also performed. The stability of individual compounds, quantified by the HPLC method, was investigated after 30 days, whereby the sample was exposed to a temperature of 40 °C. Drying efficiency was 94.68%, while TPC and TFC were 113.22 mg gallic acid/g and 28.16 mg catechin/g od FHE, respectively. The most dominant individual compounds were naringenin (22.47 mg/g) and kaempferol (21.47 mg/g) of FHE. The DSC method confirmed the FHE stability, and the SEM analysis confirmed that the extract was successfully encapsulated, without visible deformations. The obtained powder showed excellent stability in terms of the content of the dominant individual compounds, with increasing of their content after 30 days.
PB  - Belgrade : Institute of Technical Sciences of SASA
C3  - Programme and the Book of Abstracts / Twentieth Young Researchers' Conference Materials Science and Engineering, November 30 - December 2, 2022, Belgrade, Serbia
T1  - Bioactives preservation of everlasting (Helichrysum plicatum L.) flowers extract by freeze drying method and powder characterisation
SP  - 13
EP  - 13
UR  - https://hdl.handle.net/21.15107/rcub_dais_13503
ER  - 

@conference{
author = "Mutavski, Zorana and Ćujić-Nikolić, Nada and Radan, Milica and Bigović, Dubravka and Marković, Smilja and Šavikin, Katarina",
year = "2022",
abstract = "Everlasting flowers (Helichrysum plicatum L.), traditionally used for gastrointestinal disorders such as abdominal pain, jaundice, and hepatic disorders are a rich source of sensitive polyphenolic compounds whose preservation is of great importance. A critical point in the development of formulations with bioactive phenolic compounds, especially liquid extracts is their limited stability at elevated temperatures, pH variations, exposure to oxygen, light, and moisture. In order to overcome the extract limitations, drying method could be the optimal technique for preservation of bioactive compounds, in order to obtain stable powders with appropriate characteristics. One of the most advanced techniques based on the phenomenon of sublimation is a freeze drying, which enabling the long-term preservation of heat-sensitive compounds. In this study, extract obtained by percolation method was lyophilized by freeze drying method (firstly extract was frozen at -80 oC for 1 h, then freeze- dried at -60 oC with pressure of 0.011 mbar for 24 h, and finally main dried at -60 oC with pressure of 0.0012 mbar, for an additional hour in order to remove the capillary water residues). The obtained freeze-dried extract (FHE) was characterized by drying efficiency, the contents of total polyphenols-TPC and flavonoids-TFC. The most dominant polyphenolic compounds were determined and quantified by HPLC method. Differential scanning calorimetry (DSC) and scanning electron microscopy (SEM) analyzes were also performed. The stability of individual compounds, quantified by the HPLC method, was investigated after 30 days, whereby the sample was exposed to a temperature of 40 °C. Drying efficiency was 94.68%, while TPC and TFC were 113.22 mg gallic acid/g and 28.16 mg catechin/g od FHE, respectively. The most dominant individual compounds were naringenin (22.47 mg/g) and kaempferol (21.47 mg/g) of FHE. The DSC method confirmed the FHE stability, and the SEM analysis confirmed that the extract was successfully encapsulated, without visible deformations. The obtained powder showed excellent stability in terms of the content of the dominant individual compounds, with increasing of their content after 30 days.",
publisher = "Belgrade : Institute of Technical Sciences of SASA",
journal = "Programme and the Book of Abstracts / Twentieth Young Researchers' Conference Materials Science and Engineering, November 30 - December 2, 2022, Belgrade, Serbia",
title = "Bioactives preservation of everlasting (Helichrysum plicatum L.) flowers extract by freeze drying method and powder characterisation",
pages = "13-13",
url = "https://hdl.handle.net/21.15107/rcub_dais_13503"
}

Mutavski, Z., Ćujić-Nikolić, N., Radan, M., Bigović, D., Marković, S.,& Šavikin, K.. (2022). Bioactives preservation of everlasting (Helichrysum plicatum L.) flowers extract by freeze drying method and powder characterisation. in Programme and the Book of Abstracts / Twentieth Young Researchers' Conference Materials Science and Engineering, November 30 - December 2, 2022, Belgrade, Serbia
Belgrade : Institute of Technical Sciences of SASA., 13-13.
https://hdl.handle.net/21.15107/rcub_dais_13503

Mutavski Z, Ćujić-Nikolić N, Radan M, Bigović D, Marković S, Šavikin K. Bioactives preservation of everlasting (Helichrysum plicatum L.) flowers extract by freeze drying method and powder characterisation. in Programme and the Book of Abstracts / Twentieth Young Researchers' Conference Materials Science and Engineering, November 30 - December 2, 2022, Belgrade, Serbia. 2022;:13-13.
https://hdl.handle.net/21.15107/rcub_dais_13503 .

Mutavski, Zorana, Ćujić-Nikolić, Nada, Radan, Milica, Bigović, Dubravka, Marković, Smilja, Šavikin, Katarina, "Bioactives preservation of everlasting (Helichrysum plicatum L.) flowers extract by freeze drying method and powder characterisation" in Programme and the Book of Abstracts / Twentieth Young Researchers' Conference Materials Science and Engineering, November 30 - December 2, 2022, Belgrade, Serbia (2022):13-13,
https://hdl.handle.net/21.15107/rcub_dais_13503 .

TY  - CONF
AU  - Ćujić-Nikolić, Nada
AU  - Jovanović, Miloš
AU  - Drinić, Zorica
AU  - Bigović, Dubravka
AU  - Marković, Smilja
AU  - Radan, Milica
AU  - Šavikin, Katarina
PY  - 2022
UR  - https://dais.sanu.ac.rs/123456789/13681
AB  - Research hypothesis: Everlasting flowers (genus Helichrysum) represent a significant source of pharmacologically active secondary metabolites (flavonoids naringenin, kaempferol, apigenin) related to proven spasmolytic, antioxidant, and antimicrobial activity. A critical point in development of polyphenol rich extracts of H. plicatum is their limited stability, which can be solved using microencapsulation technique spray drying. Method : Helichrysum flower extract was spray dried using four different carriers, and their combinations. Besides the conventional ones (maltodextrin-MD, whey protein-WP, 20%, w/w), innovative carriers, cyclodextrins (beta-cyclodextrin-BCD, hydroxy-propyl-betacyclodextrin- HPCD, 15%, w/w) have been proposed to overcome the extract limitations. The liquid feed was spray dried in a Labtex ESDTi spray dryer, under following conditions: inlet 130  } 5°C and outlet 70  } 5°C temperatures, spraying air flow rate (75 m3/h), liquid feed (11 mL/min rate), atomization pressure (2 bar). The spray-dried Helichrysum extract (HE) was obtained and used for further analyses: total polyphenols and flavonoids contents, spectrophotometrically and individual components by HPLC method. The dried extracts were stored in brown glass tubes for 6 months under room temperature in order to determine changes in the content of total and individual compounds during period of real storage. Samples were placed at in stability chamber (Memmert, Schwabach, Germany), in the absence of light, during one month in order to determine the effect of storage during accelerated stability test. All experiments were executed in triplicates. One-way ANOVA was conducted to test the individual factors AND Duncan post hoc test for differences between the mean values detection (STATISTICA v.7.0.3, MS Office Excel v. 2010). Results : Obtained powders manifested high encapsulation efficiency (more than 80%), confirming spray drying as adequate microencapsulation technique. Spray dried HE, without a carrier addition, exhibited 97.32% and powders microencapsulated using carriers ranged from 80.07 (HE+HPCD+MD) to 96.45% (HE+HPCD) of EE%, suggesting HEs active compounds are successfully microencapsulated into examined carriers. Spray-dried HE exhibited 106.32 mg GAE/g of polyphenol content, and powders produced using different polymers ranged from 83.25 (HE+HPCD+WP) to 100.28 mg GAE/g (HE+HPCD). The highest total flavonoids content was achieved in spray-dried HE. Among powders obtained using carriers, total flavonoids ranged from 15.66 (HE+HPCD+WP) to 21.55 (HE+HPCD) mg catechin/g. HPCD complexes exhibited the highest polyphenols and flavonoids content. Results of HPLC method confirmed that mainly presented flavonoids in obtained powders were naringenin, kaempferol, quercitrin, isoquercitrin, apigenin, and apigenin and naringenin derivates. Kaempferol-3-O-glycoside was the most dominant compound presented in all tested samples. Analysis of total polyphenols, flavonoids and individual compounds were carried after one month of accelerated and 6 months of real storage conditions. After one-month, total polyphenols and flavonoids increased in all examined samples. During the accelerated storage, water migrate from CDs and other carrier complexes, resulting the higher concentration. After 6 months, total polyphenols and flavonoids increased compared to the contents before storage tests, while decreased compared to 30 days without statistical significance. Content of individual compounds did not decrease significantly after 6 months, indicating that process of spray drying was suitable for stabilization of HE active compounds and indicating good preservation using polymers. Discussion : Spray drying of Helichrysum flower extract to obtain powders with high retention of bioactive compounds was evaluated. All microencapsulated bioactive principles reached high content and preservation during storage, based on good preservation. This could be important for further use in pharmaceutical and food industry due to its confirmed health benefits.
PB  - International Association for Food Protection
C3  - Abstract Book / 7th International Food Safety Congress, 3-4 November 2022, Istanbul - Тürkiye, Grand Cevahir Hotel & Convention Center
T1  - Successful Preservation of Helichrysum plicatum L. Flowers Extract Using Novel Carriers by Spray Drying Method
UR  - https://hdl.handle.net/21.15107/rcub_dais_13681
ER  - 

@conference{
author = "Ćujić-Nikolić, Nada and Jovanović, Miloš and Drinić, Zorica and Bigović, Dubravka and Marković, Smilja and Radan, Milica and Šavikin, Katarina",
year = "2022",
abstract = "Research hypothesis: Everlasting flowers (genus Helichrysum) represent a significant source of pharmacologically active secondary metabolites (flavonoids naringenin, kaempferol, apigenin) related to proven spasmolytic, antioxidant, and antimicrobial activity. A critical point in development of polyphenol rich extracts of H. plicatum is their limited stability, which can be solved using microencapsulation technique spray drying. Method : Helichrysum flower extract was spray dried using four different carriers, and their combinations. Besides the conventional ones (maltodextrin-MD, whey protein-WP, 20%, w/w), innovative carriers, cyclodextrins (beta-cyclodextrin-BCD, hydroxy-propyl-betacyclodextrin- HPCD, 15%, w/w) have been proposed to overcome the extract limitations. The liquid feed was spray dried in a Labtex ESDTi spray dryer, under following conditions: inlet 130  } 5°C and outlet 70  } 5°C temperatures, spraying air flow rate (75 m3/h), liquid feed (11 mL/min rate), atomization pressure (2 bar). The spray-dried Helichrysum extract (HE) was obtained and used for further analyses: total polyphenols and flavonoids contents, spectrophotometrically and individual components by HPLC method. The dried extracts were stored in brown glass tubes for 6 months under room temperature in order to determine changes in the content of total and individual compounds during period of real storage. Samples were placed at in stability chamber (Memmert, Schwabach, Germany), in the absence of light, during one month in order to determine the effect of storage during accelerated stability test. All experiments were executed in triplicates. One-way ANOVA was conducted to test the individual factors AND Duncan post hoc test for differences between the mean values detection (STATISTICA v.7.0.3, MS Office Excel v. 2010). Results : Obtained powders manifested high encapsulation efficiency (more than 80%), confirming spray drying as adequate microencapsulation technique. Spray dried HE, without a carrier addition, exhibited 97.32% and powders microencapsulated using carriers ranged from 80.07 (HE+HPCD+MD) to 96.45% (HE+HPCD) of EE%, suggesting HEs active compounds are successfully microencapsulated into examined carriers. Spray-dried HE exhibited 106.32 mg GAE/g of polyphenol content, and powders produced using different polymers ranged from 83.25 (HE+HPCD+WP) to 100.28 mg GAE/g (HE+HPCD). The highest total flavonoids content was achieved in spray-dried HE. Among powders obtained using carriers, total flavonoids ranged from 15.66 (HE+HPCD+WP) to 21.55 (HE+HPCD) mg catechin/g. HPCD complexes exhibited the highest polyphenols and flavonoids content. Results of HPLC method confirmed that mainly presented flavonoids in obtained powders were naringenin, kaempferol, quercitrin, isoquercitrin, apigenin, and apigenin and naringenin derivates. Kaempferol-3-O-glycoside was the most dominant compound presented in all tested samples. Analysis of total polyphenols, flavonoids and individual compounds were carried after one month of accelerated and 6 months of real storage conditions. After one-month, total polyphenols and flavonoids increased in all examined samples. During the accelerated storage, water migrate from CDs and other carrier complexes, resulting the higher concentration. After 6 months, total polyphenols and flavonoids increased compared to the contents before storage tests, while decreased compared to 30 days without statistical significance. Content of individual compounds did not decrease significantly after 6 months, indicating that process of spray drying was suitable for stabilization of HE active compounds and indicating good preservation using polymers. Discussion : Spray drying of Helichrysum flower extract to obtain powders with high retention of bioactive compounds was evaluated. All microencapsulated bioactive principles reached high content and preservation during storage, based on good preservation. This could be important for further use in pharmaceutical and food industry due to its confirmed health benefits.",
publisher = "International Association for Food Protection",
journal = "Abstract Book / 7th International Food Safety Congress, 3-4 November 2022, Istanbul - Тürkiye, Grand Cevahir Hotel & Convention Center",
title = "Successful Preservation of Helichrysum plicatum L. Flowers Extract Using Novel Carriers by Spray Drying Method",
url = "https://hdl.handle.net/21.15107/rcub_dais_13681"
}

Ćujić-Nikolić, N., Jovanović, M., Drinić, Z., Bigović, D., Marković, S., Radan, M.,& Šavikin, K.. (2022). Successful Preservation of Helichrysum plicatum L. Flowers Extract Using Novel Carriers by Spray Drying Method. in Abstract Book / 7th International Food Safety Congress, 3-4 November 2022, Istanbul - Тürkiye, Grand Cevahir Hotel & Convention Center
International Association for Food Protection..
https://hdl.handle.net/21.15107/rcub_dais_13681

Ćujić-Nikolić N, Jovanović M, Drinić Z, Bigović D, Marković S, Radan M, Šavikin K. Successful Preservation of Helichrysum plicatum L. Flowers Extract Using Novel Carriers by Spray Drying Method. in Abstract Book / 7th International Food Safety Congress, 3-4 November 2022, Istanbul - Тürkiye, Grand Cevahir Hotel & Convention Center. 2022;.
https://hdl.handle.net/21.15107/rcub_dais_13681 .

Ćujić-Nikolić, Nada, Jovanović, Miloš, Drinić, Zorica, Bigović, Dubravka, Marković, Smilja, Radan, Milica, Šavikin, Katarina, "Successful Preservation of Helichrysum plicatum L. Flowers Extract Using Novel Carriers by Spray Drying Method" in Abstract Book / 7th International Food Safety Congress, 3-4 November 2022, Istanbul - Тürkiye, Grand Cevahir Hotel & Convention Center (2022),
https://hdl.handle.net/21.15107/rcub_dais_13681 .