• Title/Summary/Keyword: UPLC

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Chemical transformation and target preparation of saponins in stems and leaves of Panax notoginseng

  • Wang, Ru-Feng;Li, Juan;Hu, Hai-Jun;Li, Jia;Yang, Ying-Bo;Yang, Li;Wang, Zheng-Tao
    • Journal of Ginseng Research
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    • v.42 no.3
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    • pp.270-276
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    • 2018
  • Background: Notoginsenoside Ft1 is a promising potential candidate for cardiovascular and cancer disease therapy owing to its positive pharmacological activities. However, the yield of Ft1 is ultralow utilizing reported methods. Herein, an acid hydrolyzing strategy was implemented in the acquirement of rare notoginsenoside Ft1. Methods: Chemical profiles were identified by ultraperformance liquid chromatography coupled with quadruple-time-of-flight and electrospray ionization mass spectrometry (UPLC-Q/TOF-ESI-MS). The acid hydrolyzing dynamic changes of chemical compositions and the possible transformation pathways of saponins were monitored by ultrahigh-performance LC coupled with tandem MS (UHPLC-MS/ MS). Results and conclusion: Notoginsenoside Ft1 was epimerized from notoginsenoside ST4, which was generated through cleaving the carbohydrate side chains at C-20 of notoginsenosides Fa and Fc, and vinaginsenoside R7, and further converted to other compounds via hydroxylation at C-25 or hydrolysis of the carbohydrate side chains at C-3 under the acid conditions. High temperature contributed to the hydroxylation reaction at C-25 and 25% acetic acid concentration was conducive to the preparation of notoginsenoside Ft1. C-20 epimers of notoginsenoside Ft1 and ST4 were successfully separated utilizing solvent method of acetic acid solution. The theoretical preparation yield rate of notoginsenoside Ft1 was about 1.8%, which would be beneficial to further study on its bioactivities and clinical application.

Antioxidant activities of ethanol extracts from barley sprouts (새싹보리 에탄올 농도별 추출물의 산화방지 활성)

  • Chae, Kyu Seo;Ryu, Eun Hye;Kim, Ki Deok;Kim, Yong-Suk;Kwon, Ji Wung
    • Korean Journal of Food Science and Technology
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    • v.51 no.5
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    • pp.486-491
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    • 2019
  • Phenolic compounds and antioxidant activities of ethanol extracts from barley sprouts were evaluated in this study. Barley sprouts were extracted using water and ethanol in various concentration (25, 50, and 75%) using reflux extraction methods. Ultra performance liquid chromatography (UPLC) analysis showed that barley sprouts are mainly composed of rutin, gallic acid, ferulic acid, and ${\rho}$-coumaric acid. The 75% ethanol extracts had higher total polyphenol contents ($44.01{\pm}1.32mg/g$) and total flavonoid contents ($102.96{\pm}2.49mg/g$). 2,2-diphenyl-1-picrylhydrazyl radical scavenging activity ($EC_{50}$ value: $1.65{\pm}0.02mg/mL$) and 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) diammonium salt radical scavenging activity ($EC_{50}$ value: $1.67{\pm}0.02mg/mL$) of the 75% ethanol extracts of barley sprouts were found to be the most effective. The 75% ethanol extracts of barley sprouts exhibited a strong reducing activity and ferric reducing antioxidant activity. As a result, the 75% ethanol extracts of barley sprouts showed stronger antioxidant activity than other extracts.

Anti-inflammatory effects of ethyl acetate fraction of unripe astringent persimmon (Diospyros kaki Thunb. cv. Cheongdo-Bansi) on lipopolysaccharide-stimulated RAW 264.7 cells (지방질다당류로 자극한 RAW 264.7 세포에서 청도반시 땡감 에틸 아세테이트 분획물의 항염증 효과)

  • Park, Ye Bin;Jeong, Ha-Ram;Lee, Seung Hwan;Kim, Taewan;Kim, Dae-Ok
    • Korean Journal of Food Science and Technology
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    • v.51 no.1
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    • pp.90-96
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    • 2019
  • Unripe astringent persimmon (Diospyros kaki Thunb. cv. Cheongdo-Bansi) is a by-product produced when thinning out the superfluous fruit of persimmon. We investigated whether unripe astringent persimmon has antioxidative and anti-inflammatory effects. Unripe astringent persimmon extract was fractionated sequentially in n-hexane, chloroform, ethyl acetate, n-butanol, and water. The ethyl acetate fraction had the highest total phenolic content, total flavonoid content, and antioxidant capacity compared to those of the other fractions. Pretreatment of lipopolysaccharide-stimulated RAW 264.7 macrophages with the ethyl acetate fraction reduced nitric oxide, interleukin-6, and intracellular oxidative stress in a dose-dependent manner. Ultra-high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry analysis revealed gallic acid, protocatechuic acid, 4-hydroxybenzoic acid, quercetin-3-O-glucoside, quercetin, and p-coumaric acid as the phenolic compounds of the ethyl acetate fraction. Collectively, these findings suggest that unripe astringent persimmon is a source of functional materials that can promote antioxidative and anti-inflammatory effects.

Enrichment of Short-Chain Ceramides and Free Fatty Acids in the Skin Epidermis, Liver, and Kidneys of db/db Mice, a Type 2 Diabetes Mellitus Model

  • Kim, Minjeong;Jeong, Haengdueng;Lee, Buhyun;Cho, Yejin;Yoon, Won Kee;Cho, Ahreum;Kwon, Guideock;Nam, Ki Taek;Ha, Hunjoo;Lim, Kyung-Min
    • Biomolecules & Therapeutics
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    • v.27 no.5
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    • pp.457-465
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    • 2019
  • Patients with diabetes mellitus (DM) often suffer from diverse skin disorders, which might be attributable to skin barrier dysfunction. To explore the role of lipid alterations in the epidermis in DM skin disorders, we quantitated 49 lipids (34 ceramides, 14 free fatty acids (FFAs), and cholesterol) in the skin epidermis, liver, and kidneys of db/db mice, a Type 2 DM model, using UPLC-MS/MS. The expression of genes involved in lipid synthesis was also evaluated. With the full establishment of hyperglycemia at the age of 20 weeks, remarkable lipid enrichment was noted in the skin of the db/db mice, especially at the epidermis and subcutaneous fat bed. Prominent increases in the ceramides and FFAs (>3 fold) with short or medium chains ($LXR{\alpha}/{\beta}$ and $PPAR{\gamma}$, nuclear receptors promoting lipid synthesis, lipid synthesis enzymes such as elongases 1, 4, and 6, and fatty acid synthase and stearoyl-CoA desaturase were highly expressed in the skin and livers of the db/db mice. Collectively, our study demonstrates an extensive alteration in the skin and systemic lipid profiles of db/db mice, which could contribute to the development of skin disorders in DM.

Survey of Mycotoxin Contamination in Grains and Grain Products (곡류 및 곡류가공품 중 곰팡이독소 오염도 조사 연구)

  • Yang, Yongshik;Lee, Hyang Hee;Kim, Ae Gyeong;Ryu, Keun Young;Choi, Su Yeon;Seo, Doo Ri;Seo, Kye Won;Cho, Bae Sik
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.205-211
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    • 2019
  • This study surveyed mycotoxin contamination in grains and grain products, which were purchased from supermarkets and traditional markets from October 2017 to September 2018 in Gwangju (Metropolitan City). A total of 127 samples including adlay, sorghum, millet, rice, oats, barley, buckwheat, corn as grains, and rice flour, buckwheat flour, roasted barley and corn, as grain products were surveyed. The tested mycotoxins were aflatoxin ($AFB_1$, $AFB_2$, $AFG_1$, $AFG_2$), fumonisin ($FUB_1$, $FUB_2$), ochratoxin A (OTA), and zearalenone (ZON). Mycotoxins were analyzed simultaneously with a UPLC-tandem mass spectrometry method. Fumonisin ($B_1+B_2$) was detected at the range of $4.8{\sim}738.5{\mu}g/kg$ in 35 samples and zearalenone at $8.4{\sim}507.6{\mu}g/kg$ in 20 samples, respectively. No other mycotoxins were detected. Risk assessment was evaluated by using estimated daily intake (EDI) and provisional maximum tolerable daily intake (PMTDI) in accordance with the Joint FAO/WHO Expert Committee on Food Additives (JECFA). When the hazard index (HI) was expressed as $(EDI/PMTDI){\times}100$, the HI (%) showed in the range of 0.0019~1.9526%. Based on these results, mycotoxin concentrations in the grains and grain products were within safe levels.

Variation in Fatty Acid Composition, Caffeic and Rosmarinic Acid Content, and Antioxidant Activity of Perilla Accessions (들깨 유전자원의 지방산 변이 및 rosmarinic acid와 caffeic acid의 함량에 따른 항산화 활성 비교)

  • Kim, Da Jeong;Assefa, Awraris Derbie;Jeong, Yi Jin;Jeon, Young Ah;Lee, Jae Eun;Lee, Myeong Chul;Lee, Ho Sun;Rhee, Ju Hee;Sung, Jung Sook
    • Korean Journal of Medicinal Crop Science
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    • v.27 no.2
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    • pp.96-107
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    • 2019
  • Background: The aim of this study was to compare the fatty acid composition, antioxidant activity, and the content of two major phenolic acids, caffeic and rosmarinic acids, of 45 Perilla accessions collected from Russia. Methods and Results: A total of 45 accessions of the genus Perilla were used in this study. The antioxidant activities of these accessions were analyzed using a spectrophotometer, and their caffeic and rosmarinic acid contents were determined using a reversed-phase ultraperformance liquid chromatography (UPLC) system. The Perilla seed oil was recovered using hexane in a soxhlet extraction method. The fatty acid compositions were analyzed using a Shimadzu QP2010 gas chromatography-mass spectoroscopy system. The results showed that accessions IT226732 and IT274300 had the highest content of caffeic and rosmarinic acid, respectively. A cluster analysis based on antioxidant assay results and concentration of phenolic acids led to the categorization of Perilla accessions into three major groups. The accessions in Group I were characterized by higher caffeic and rosmarinic acid content and antioxidant activity, compared to the accessions in the other two groups (p < 0.05). The total oil content ranged between 28.39 and 46.89%. The compositions of oleic, linoleic, and linolenic acid ranged from 11.83 to 19.55%, 11.92 to 16.71%, and 59.19 to 67.28%, respectively. Conclusions: The results of this study indicated that accessions IT274300, IT226732, IT274293, IT235818, and IT235820 could be used as a source of functional materials.

Chemical profile and antioxidant activity of peel of Yellowball, a novel citrus variety

  • Sun Lee;Seong-Ho Jo;Ji-Hyun An;Seong-man Jeong;Dong-Shin Kim;Sang Suk Kim;Suk Man Park;Su Hyun Yun;Seung-Gab Han;Hyun-Jin Kim
    • Food Science and Preservation
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    • v.30 no.2
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    • pp.235-246
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    • 2023
  • Yellowball (Citrus hybrid cv. Yellowball ) is a new citrus hybrid between Haruka (C. tamurana × natsudaidai ) and Kiyomi (C. unshiu × sinensis) and is known to possess strong antioxidant activity. However, detailed information on the antioxidant components of its peel has not yet been reported. This study evaluated the antioxidant activity of the peel and identified the antioxidant components by fractionating a methanolic extract of Yellowball peels using liquid-liquid extraction with n-hexane, ethyl ether (ether), ethyl acetate (EA), butanol, and water. The phenolic contents and antioxidant activities of the n-hexane, ether, and EA fractions were higher than those of the other fractions, and these fractions were further separated by semi-preparative high-performance liquid chromatography (HPLC). Four antioxidant peaks, EA1, EA2, EA3, and He1, were isolated and analyzed using ultra-performance liquid chromatography-quadrupole-time- of-flight mass spectrometry (UPLC-Q-TOF MS). Sinapoyl glucoside and hesperidin were identified in EA2 and EA3, respectively, and a polymethoxylated flavone (PMF) complex (5-hydroxy-3,6,7,8,3',4'-hexamethoxyflavone, natsudaidain, tetrameth- oxyflavone, and tangeretin) was identified in He1. A compound in EA1 with m/z 223.0246 [M-H] could not be identified and was named unknown2. The antioxidant activity of unknown2 (IC50=69.17 ㎍/mL) was similar to that of Trolox, which was noted as a major antioxidant in Yellowball peel. Further studies on the antioxidant capacity of Yellowball peel are required; however, these results provide a foundation for using Yellowball peel as an antioxidant.

Characterization of Antibacterial Compounds from Bacillus polyfermenticus CJ6 and Its Growth Inhibition Effect on Food-Borne Pathogens (Bacillus polyfermenticus CJ6가 생산하는 항세균 물질의 특성 및 병원성 식중독 미생물의 성장 억제 효과)

  • Jung, Ji-Hye;Chang, Hae-Choon
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.40 no.6
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    • pp.903-911
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    • 2011
  • In this study, Bacillus polyfermenticus CJ6 harboring antibacterial activity was isolated from meju. The antibacterial activity of Bacillus polyfermenticus CJ6 was stable in the pH range of 3.0~9.0, but it disappeared after culture at $70^{\circ}C$ for 24 hr. Antibacterial activity was inactivated by proteinase K, protease, and ${\alpha}$-chymotrypsin, indicating its proteinaceous nature. The growth inhibitory effects of B. polyfermenticus CJ6 culture on food-borne pathogens such as Staphylococcus aureus, Salmonella Typhi, Listeria monocytogenes, and Escherichia coli O157:H7 were examined in this study. Approximately 6~6.2 log CFU/mL of each pathogen was co-cultured with B. polyfermenticus CJ6 in a 50 mL culture volume for 24 hr. Growth of S. aureus and L. monocytogenes was completely inhibited after 3 hr of incubation. Growth of S. Typhi and E. coli O157:H7 was also completely inhibited after 6 hr of incubation. The antibacterial compounds from B. polyfermenticus CJ6 were purified by solid phase extraction (C18 Sep-pak cartridge), recycling preparative HPLC, and analytical HPLC. Ultra-high performance liquid chromatography and electrospray ionization tandem mass spectrometry analysis were used to identify the purified antibacterial compounds, which were confirmed to be five peptides (757.4153 Da, 750.3444 Da, 1024.5282 Da, 1123.6083 Da, and 1617.8170 Da).

Metabolites profiling and hypolipidemic/hypocholesterolemic effects of persimmon (Diosyros kaki Thumb.) by different processing procedures: in vitro and in vivo studies (제조방법에 따른 떫은감 (Diosyros kaki Thumb.)의 대사체 프로파일링과 중성지질/콜레스테롤 대사 관련 유전자발현 연구 : in vitro 및 in vivo 연구)

  • Park, Soo-Yeon;Oh, Eun-Kyung;Lim, Yeni;Shin, Ji-Yoon;Jung, Hee-Ah;Park, Song-Yi;Lee, Jin Hee;Choe, Jeong-Sook;Kwon, Oran
    • Journal of Nutrition and Health
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    • v.51 no.4
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    • pp.275-286
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    • 2018
  • Purpose: Our previous study demonstrated that persimmon (Diospyros kaki Thumb.) at different stages of ripening provided different protective effects against high-fat/cholesterol diet (HFD)-induced dyslipidemia in rats. In this study, we compared the metabolites profile and gene expressions related to triglyceride (TG)/cholesterol metabolism in vitro and in vivo after treating with persimmon water extracts (PWE) or tannin-enriched persimmon concentrate (TEP). Methods: Primary and secondary metabolites in test materials were determined by GC-TOF/MS, UHPLC-LTQ-ESI-IT-MS/MS, and UPLC-Q-TOF-MS. The expression of genes related to TG and cholesterol metabolism were determined by RT-PCR both in HepG2 cells stimulated by oleic acid/palmitic acid and in liver tissues obtained from Wistar rats fed with HFD and PWE at 0, 150, 300, and 600 mg/d (experiment I) or TEP at 0, 7, 14, and 28 mg/d (experiment II) by oral gavage for 9 weeks. Results: PLS-DA analysis and heatmap analysis demonstrated significantly differential profiling of metabolites of PWE and TEP according to processing of persimmon powder. In vitro, TEP showed similar hypolipidemic effects as PWE, but significantly enhanced hypocholesterolemic effects compared to PWE in sterol regulatory element-binding protein 2 (SREBP2), HMG-CoA reductase (HMGCR), proprotein convertase subtilisin/kexin type 9 (PCSK9), cholesterol $7{\alpha}-hydroxylase$ (CYP7A1), and low density lipoprotein receptor (LDLR) gene expression. Consistently, TEP and PWE showed similar hypolipidemic capacity in vivo, but significantly enhanced hypocholesterolemic capacity in terms of SREBP2, HMGCR, and bile salt export pump (BSEP) gene expression. Conclusion: These results suggest that column extraction after hot water extraction may be a good strategy to enhance tannins and long-chain fatty acid amides, which might cause stimulation of hypocholesterolemic actions through downregulation of cholesterol biosynthesis gene expression and upregulation of LDL receptor gene expression.

A Study on Contact Dermatitis-Causing Substances Concentration in Commercial Oxidative Hair-Coloring Products (유통 산화형 염모제의 접촉성피부염 유발물질 함량 연구)

  • Na, Young Ran;Koo, Hee Soo;Lee, Seung Ju;Kang, Jung Mi;Jin, Seong Hyeon
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.40 no.2
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    • pp.203-214
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    • 2014
  • We measured the contact dermatitis-causing substances concentrations in 28 commercial oxidative hair-coloring products. This study was aimed to provide the fundamental data about oxidative hair-coloring products. We selected 10 oxidation dyes (p-phenylenediamine, toluene-2,5-diamine, m-phenylenediamine, nitro-p-phenylenediamine, p-aminophenol, m-aminophenol, o-aminophenol, p-methylaminophenol, N,N'-bis(2-hydroxyethyl)-p-phenylenediamine sulfate, 2-methyl-5-hydroxyethylaminophenol) and 4 heavy metal (nikel; Ni, chromium; Cr, cobalt; Co, copper; Cu) as contact dermatitis-causing substances. To identify 10 oxidation dyes, hexane-2% sodium sulfite was used for the rapid and simple extraction and ultra performance liquid chromatography (UPLC) analysis was used for simultaneous analysis in 12 minutes. 10 oxidative dyes were detected as indicated on the product packaging and each concentration was lower than prescribed upper concentration limit by pharmaceutical manufacturing standards. And we analysed inductively coupled plasma-optical emission spectrophotometer (ICP-OES) for content search of heavy metal after microwave digestion. The heavy metal average concentration in oxidative hair-coloring products was 0.572 ${\mu}g/g$ for Ni, 3.161 ${\mu}g/g$ for Cr, 2.029 ${\mu}g/g$ for Co, 0.420 ${\mu}g/g$ for Cu, respectively. The average of concentration in powder type (henna) was higher than those of other foam and cream type oxidative hair-coloring products as follows; 1.800 ${\mu}g/g$ for Ni, 10.127 ${\mu}g/g$ for Cr, 7.082 ${\mu}g/g$ for Co, 1.451 ${\mu}g/g$ for Cu. Hair coloring products were classified into the six colors - black, dark brown, brown, dark brown, light brown, red brown and analyzed. Brown color had the highest average concentration of Co and the others had the highest average concentration of Cr.