• Title/Summary/Keyword: Trifluoroacetic acid

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Analytical Method Development of Isoscoparin in Silene seoulensis Extract Using HPLC (HPLC 를 이용한 가는장구채 추출물의 Isoscoparin 분석법 개발)

  • Kwon, Jin Gwan;Seo, Changon;Jung, Yeon Woo;Choi, Yongmun;Shin, Hyun Tak;Jung, Su Young;Choi, Jeong June;Kim, Jin Kyu
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.47 no.1
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    • pp.57-63
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    • 2021
  • In this study, isoscoparin was selected as an indicator component to develop Silene seoulensis extract as a functional cosmetic material, and we developed an analysis method using high performance liquid chromatography (HPLC) for quality control. HPLC was performed on a Unison US-C18 with a gradient elution of 0.05% (v/v) trifluoroacetic acid (TFA) and methanol at a flow rate of 1.0 mL/min at 35 ℃, and the detection wavelength was 330 nm. The HPLC method was performed in accordance with the international conference on harmonization (ICH) guideline (version 4, 2005) of analytical procedures with respect to specificity, precision, accuracy, and linearity. The limits of detection and quantitation were 0.02 and 0.07 mg/mL respectively. Calibration curves showed good linearity (R2 > 0.99988), and the precision of analysis was satisfied (less than 0.46%). In addition, the recovery rate was in the range of 99.10 to 101.61%, it was shown to be accurate. This result indicated that the established HPLC method is very useful for the determination of marker compounds in Silene seoulensis extracts.

Simultaneous Determination of Eight Compounds in Lysimachia christinae by HPLC-DAD

  • Gahee Ryu;Choong Je Ma
    • Natural Product Sciences
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    • v.28 no.4
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    • pp.187-193
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    • 2022
  • Lysimachia christinae Hance was commonly used in Oriental medicine for treating the hepatitis virus, cholecystitis and cholagogic efficiency. According to the previous study, it possesses high antioxidant and anti-inflammatory activity. Simultaneous determination analytical method of isolated eight compounds, cynaroside (1), 2-(3,4-dimethoxyphenyl) ethyl O-α-L-arabinopyranosyl-(1→2)-O-[6-deoxy-α-L-mannopyranosyl-(1→3)] β-D-glucopyranoside (2), stearylester ricinoleic acid (3), (E)-4-(3,4-dimethoxyphenyl) but-3-en-1-yl palmitate (4), 2-hydroxy-24-methoxy-4-tetracosenoic acid (5), 2-hydroxy-24-propoxy-4-tetracosenoic acid (6), β-sitosterol (7), and androst-16-ene-3,6-diol (8) were established by using HPLC-DAD. This HPLC analysis was detected on a Dionex C18 column (5 ㎛, 120 Å, 4.6 mm × 150 mm) at 25℃. The mobile phase consisted of 0.1% trifluoroacetic acid and acetonitrile at a flow rate of 1 mL/min. Validation of the method was assessed by linearity, precision and accuracy test. Calibration curve was good at r2 > 0.9998. Limits of detection (LOD) ranged from 0.19 to 8.18 g/ml and Limits of quantification (LOQ) ranged from 0.19 to 24.80 g/ml. The relative standard deviations (RSD) values of precision test, intra- and inter- day, were less than 0.99% and 1.0%. The accuracy test results ranged from 98.81% to 106.49% and RSD values were less than 0.95%. These results showed that the HPLC-DAD method was very reliable and accurate for the quantity analysis of eight compounds in L. christinae extract for quality control.

Screening of Domoic Acid, a Marine Neurotoxin, in Korean Shellfishes (국내산 패류의 신경독소 domoic acid 검색)

  • Koh, Eun-Mi;Kwon, Hoon-Jeong
    • Korean Journal of Food Science and Technology
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    • v.34 no.6
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    • pp.1130-1133
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    • 2002
  • Domoic acid, and amnesic shellfish poison, is a neurotoxin frequently found in shellfishes. Guidance level for the consumable shellfish has been established as $20\;{\mu}g$ domoic acid/g by Health and Welfare Canada and U.S. FDA. Domoic acid is produced by pennate diatom, a Nitzschia pungens f. multiseries ingested by the shellfish. Content of domoic acid in shellfish samples collected along the Korean shoreline from May to December of 1999 was analyzed. The collection included 1 Gastropoda (Murex shell) and 11 Bivalvias (oyster, little neck clam, orient hard clam, venus clam, surf clam, ark shell, hard-shelled mussel, pen shell, jack-knife clam, pink butterfly shell, and granulated ark shell). Samples were homogenized, extracted with 50% methanol, filtered, and analyzed by reversed-phase liquid chromatography at 242 nm with mobile phase consisting of 10% acetonitrile and 0.1% trifluoroacetic acid. Recovery of the HPLC analysis was 95.80% (${\pm}1.09$). All tested samples showed no domoic acid at the detection limit of 50 ng/g.

Preliminary Results of Extraction, Separation and Quantitation of Arsenic Species in Food and Dietary Supplements by HPLC-ICP-MS

  • Nam, Sang-Ho;Cheng, John;Mindak, William R.;Capar, Stephen G.
    • Bulletin of the Korean Chemical Society
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    • v.27 no.6
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    • pp.903-908
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    • 2006
  • Various extraction procedures were investigated using reference materials and samples to evaluate extraction efficiency and effectiveness. Inductively coupled plasma mass spectrometry (ICP-MS) was used to measure total arsenic and to quantitate arsenic species when coupled to an HPLC (high pressure liquid chromatography). Arsenic species were extracted from rice flour (NIST SRM 1568a) with water/methanol mixtures using accelerated solvent extraction (ASE). Total arsenic extraction efficiency ranged from 42 to 64%, for water and various methanol concentrations. From spinach (NIST SRM 1570), freeze-dried apple, and rice flour (NIST SRM 1568a), arsenic species were extracted with trifluoroacetic acid (TFA) at 100 ${^{\circ}C}$. Total arsenic extraction efficiency was 90% for spinach, 75% for freeze-dried apple, and 83% for rice flour. Enzymatic extraction with alpha-amylase and sonication resulted in extraction efficiency of 104% for rice flour, 98% for freeze-dried apple, and 7% for spinach. Chromatograms of arsenic species extracted by the optimum extraction methods were obtained, and the species were quantified. Arsenite (As(III)), arsenate (As(V)), dimethylarsinic acid (DMA), and monomethylarsonic acid (MMA) were found in the apple sample, and DMA and As(V) in the rice flour sample. As(V) and MMA were found in three herbal dietary supplement samples.

Determination of Veterinary Antibiotic Residues: III. Analytical Methods_A Review (시료 중 잔류 항생제 분석 방법: III. 기기 분석 방법)

  • Kim, Chansik;Ryu, Hong-Duck;Chung, Eu Gene;Kim, Yongseok;Rhew, Doug Hee
    • Journal of Korean Society on Water Environment
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    • v.32 no.6
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    • pp.649-669
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    • 2016
  • This study explored the analytical conditions for 21 veterinary antibiotics which have been popularly sold in South Korea in 2014 but have not yet been targeted in EPA method 1694. Most of the selected antibiotics were separated by a reverse-phase C18 column with a combination of (buffered) water and organic polar solvent, which was commonly methanol and acetonitrile in the gradient elution mode. Volatile additives such as formic acid, ammonium acetate and ammonium formate were usually added to the mobile phases to minimize asymmetrical and tailing of antibiotics' peaks and to increase their ionization in mass spectrometry. The analytical methods of aminoglycoside antibiotics were distinct from those of the other antibiotics in terms of adoption of ion-pair chromatography (IPC) and hydrophilic interaction liquid chromatography (HILIC) capable of retaining and separating extremely polar compounds due to their hydrophilicity. Trifluoroacetic acid or heptafluorobutyric acid was frequently added to the mobile phase as an ion-pair reagent for the IPC. Tandem mass spectrometry was numerously applied to the detection of antibiotics using positive electrospray ionization (ESI) and the selected reaction monitoring (SRM) mode. All reviewed analytical methods had been/were validated by evaluating recovery, limits of detection and quantification, decision limit or detection capability of the methods.

Isolation of Peptides from Human Blood by RP-HPLC (RP-HPLC를 이용한 혈액에 포함된 펩타이드의 분리)

  • ;;Yulia Polyakova
    • KSBB Journal
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    • v.17 no.3
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    • pp.261-265
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    • 2002
  • The biologically active peptides in human blood can adjust the functions of many physiological systems. The peptides in human blood were separated on the five steps of linear gradient-elution mode by RP-HPLC with UV detection. The size of commercially available $C_{18}$ chromatographic column was 4.60$\times$150 mm with particle size of 5 $\mu\textrm{m}$ and pore size of 100 $\AA$. The mobile phases used were water in 0.75% trifluoroacetic acids (TFA) and organic modifier of acetonitrile. The isolation methods suggested in this work for peptides from the blood were composed of the formation of immiscible liquid layers and precipitation by centrifuge and chemicals of sodium citrate and trichloroacetic acid (TCA). The some peptides were identified based on the retention times previously constructed database.

Neutral and Amino Sugars Composition of a Lectin from Maackia fauriei (Maackia fauriei 유래 렉틴의 중성당 및 아미노당 조성)

  • Na, Kwang-Heum;Park, Byung-Tae;Park, Jae-Wan;Han, Kyong-Jin;Park, Hyun-Joo;Kim, Ha-Hyung
    • YAKHAK HOEJI
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    • v.53 no.1
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    • pp.34-40
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    • 2009
  • The glycosylation of therapeutic glycoproteins can affect their efficacy, stability, solubility, and half-life. Analyzing the composition of monosaccharides, such as that of neutral and amino sugars, is the first step for elucidating the structure of glycan attached to glycoproteins. In the present study, neutral and amino sugars of lectin obtained from Maackia fauriei were analyzed using an enzyme-linked lectinsorbent assay (ELLA) and high-performance anion exchange chromatography with pulsed amperometric detection (HPAEC-PAD). Peroxidase-labeled lectins such as concanavalin A, Ricinus communis agglutinin, and soybean agglutinin were used for ELLA, since they specifically bind to the monosaccharide residue most frequently encountered in a glycan. The hydrosylate of lectin was prepared by treatment with trifluoroacetic acid, which resulted in the lectin mainly possessing the N-glycan consisting of 98.1 pmol Fuc, 342.1 pmol GlcN, 51.9 pmol Gal, 678.9 pmol Man, and 330.7 pmol Xyl. The present results demonstrate that ELLA and HPAEC-PAD are very effective methods for rapidly estimating the types and relative amounts of monosaccharides in intact glycoproteins.

Purification of Progelatinase A (Matrix Metalloproteinase 2) and a Tissue Inhibitor of Metalloproteinase-2(TIMP-2) from T98G Human Glioblastoma Cells

  • Lee, Ho-Jae;Chung, Myung-Chul;Lee, Choong-Hwan;Chun, Hyo-Kon;Kho, Yung-Hee
    • BMB Reports
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    • v.28 no.1
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    • pp.33-39
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    • 1995
  • The Gelatinases (typeIV collagenases) are metalloproteinases that may play an important role in tumor invasion and metastasis. Progelatinase A was purified from a conditioned medium of T98G human glioblastoma cells. TIMP-2 complexed progelatinase A and free progelatinase A were separated by heparin affinity HPLC. The final product was homogeneous on SDS-PAGE, with a molecular weight of 64,000 daltons without reduction. TIMP-2 and free progelatinase A were separated from TIMP-2 complexed progelatinase A by reverse-phase HPLC in the presence of trifluoroacetic acid. TIMP-2 complexed progelatinase A was resistant to activation by p-aminophenyl mercuric acetate (APMA), and showed less than 20% of the activity of the TIMP-2 free active enzyme. TIMP-2 free progelatinase A was easily activated to the mature form with a molecular weight of 57,000 daltons by APMA and showed high activity compared to the TIMP-2 complexed enzyme.

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CO2 Solubilities in Amide-based Brønsted Acidic Ionic Liquids

  • Palgunadi, Jelliarko;Im, Jin-Kyu;Kang, Je-Eun;Kim, Hoon-Sik;Cheong, Min-Serk
    • Bulletin of the Korean Chemical Society
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    • v.31 no.1
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    • pp.146-150
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    • 2010
  • A distinguished class of hydrophobic ionic liquids bearing a Br${\o}$nsted acidic character derived from amide-like compounds were prepared by a neutralization reaction of N,N-diethylformamide, N,N-dibutylformamide, 1-formylpiperidine, and $\varepsilon$-caprolactam with trifluoroacetic acid and physical absorptions of $CO_2$ in these ionic liquids were demonstrated and evaluated. $CO_2$ solubilities in these ionic liquids were influenced by the molecular structure of the cation and were apparently increased with the molar volume. Comparison based on a volume unit reveals that $CO_2$ solubilities in these liquids are relatively higher than those in imidazolium-based ionic liquids. Henry's coefficients calculated from low-pressure solubility tests at 313 to 333 K were used to derive the thermodynamics quantities. Enthalpy and entropy of solvation may share equal contributions in solubility.

HPLC Study for Egg White Analysis (달걀 단백질 분석을 위한 HPLC 연구)

  • Jeon, Young-Ju;Lee, Eun;Kim, In-Ho
    • KSBB Journal
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    • v.22 no.2
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    • pp.119-122
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    • 2007
  • Since egg white contains various protein, it is important to research the protein distribution of egg white. Specially, lysozyme and ovalbumin important proteins, are used in medicine and food industry. Reversed phase high performance liquid chromatography has been used for separation of egg white, and column of RP-HPLC is available in variety. We have used C4, C8 and C18 columns to obtain chromatograms by varying carbon chain length of stationary phase. Long carbon chain length of stationary phase has good separation of egg white. Also, we have changed the composition of mobile phase (acetonitrile, water, and trifluoroacetic acid) to find optimum chromatograms. Acetonitrile and water composition of 50 : 50 show many peaks from egg white. Isocartic and gradient elution in RP-HPLC were used to compare the chromatography of egg white.