• Natural Product Sciences
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• 제21권1호
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• pp.20-24
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• 2015

Cyanidin-3-glucoside (C3G) and cyanidin-3-rutinoside (C3R) were isolated by high-performance countercurrent chromatography (HPCCC) using a two-phase solvent system composed of tert-butyl methyl ether/n-butanol/acetonitrile/water/trifluoroacetic acid (1 : 3 : 1 : 5 : 0.01, v/v) to give pure C3G (34.1 mg) and C3R (14.3 mg) from 1.5 g crude mulberry fruit extract. Using the pure C3G and C3R, a reliable high-performance liquid chromatography (HPLC) method was developed and validated to determine the C3G and C3R contents in mulberry fruit. C3G and C3R were separated simultaneously using an Eclipse XDB-C18 column ($4.6{\times}250mm$ I.D., $5{\mu}m$) coupled with a photodiode array detector (PDA). The gradient elution of the mobile phase consisting of acetonitrile (0.5% formic acid) and water (0.5% formic acid) was applied (1.0 mL/min), and the detection wavelength was 520 nm. The calibration curves of C3G and C3R showed good linearity (both with $r^2=0.9996$) in the concentration range $15.625-500{\mu}g/mL$, and the relative standard deviations (RSD%) of intra- and inter-day variability were in the ranges 2.1 - 8.2% and 4.1 - 17.1%, respectively. The accuracies were ranged 96.5 - 102.6% for C3G and C3R, respectively. The developed HPLC method was used to determine the contents of C3G and C3R in newly harvested mulberry from eight different provinces of Korea.

• Archives of Pharmacal Research
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• 제10권1호
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• pp.60-66
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• 1987

A procedure utilizing high pressure liquid chroatography coupled with UV detection is described for the determination of blood concentration of higenamine. Deproteinized serum was pretreated with$C_{18}$(Sep-pak $C_{18}$ cartridge) and the 70% EtOH eluent was applied onto a reversed-phase column ($\mu$ Bondapak $C_{18}]$) with a 15% acetonitrile in 0.05 N $NaH_2$$PO_4$-trichloroacetic acid mixed buffer (pH 2.8) as a mobile phase. With the UV detection at 232 nm, the retention times of higenamine and 1, 2, 3, 4-tetrahydropapaveroline, an internal standard, were 5.2 min and 3.9 min respectively. The blood concentration of higenamine was meausred at regular intervals after i. v. injection of higenamine to rabbit. A drastic decrease in higenamine concentration to 30% of the maximum value obtained immediately after the injection, was observed during the first 1-2 min period and thereafter the rate of decrease was slowed down. The analytical result seemed to coincide with the pharmacological effect of higenamine exerting the maximum chronotropic and hypotensive effect at the completion of the injections which were progressively recovered.

• Bulletin of the Korean Chemical Society
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• 제35권1호
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• pp.197-203
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• 2014

A rapid, accurate and precise method for the determination of 22 amino acids in Isatidis Radix by Hydrophilic Interaction Ultra-High-Performance Liquid Chromatography Coupled with Triple-Quadrupole Mass Spectrometry (HILIC-UPLC-MS/MS) was established. Chromatographic separation was carried out on a Acquity UPLC BEH Amide column ($2.1mm{\times}100mm$, $1.7{\mu}m$) with gradient elution of acetonitrile (containing 0.05% formic acid and 2 mM ammonium formate) and water (containing 0.15% formic acid and 10 mM ammonium formate) at a flow rate of 0.4 mL/min; Waters Xevo$^{TM}$ TQ worked in multiple reaction monitoring mode. All components were separated in 17 min. All calibration curves were linear ($R^2$ > 0.991) over the tested ranges. The limits of detection (LOD) and limits of quantitation (LOQ) for these compounds were 0.21-79.55 and 0.72-294.23 ng/mL, respectively. The average recoveries were in the range of 93.75-104.16% with RSD value less than 6.56%. Therefore, this method could be an alternative assay for the determination of 22 amino acids in Isatidis Radix due to its rapidness, sensitivity, less sample and solvent consumption.

• 생약학회지
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• 제46권2호
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• pp.123-132
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• 2015

In this study, we carried out quantification analysis of the six marker components, geniposidic acid, chlorogenic acid, geniposide, pinoresinol diglucoside, liriodendrin, and genipin in the 70% ethanol extracts of non-processed Eucommiae Cortex and processed Eucommiae Cortex using a high-performance liquid chromatography coupled with photodiode array detector. The six components were separated on Gemini C₁₈ column (5 μm, 4.6×250 mm) by the gradient elution with 1.0% (v/v) acetic acid in water and 1.0% (v/v) acetic acid in acetonitrile as mobile phase. The flow rate was 1.0 mL/min and the injection volume was 10 mL. The amount of geniposidic acid, chlorogenic acid, geniposide, pinoresinol diglucoside, liriodendrin, and genipin in non-processed Eucommiae Cortex were 1.31, 0.31, 0.66, 0.46, 0.46, and 0.03%, respectively, while the amount of the six compounds in non-processed Eucommiae Cortex were 0.04-0.78, 0.01-0.14%, 0.05-0.63%, 0.01-0.37%, 0.15-0.42%, and not detected, respectively. After processing treatment, the contents of three iridoids, two lingnan, and one phenylpropanoid decreased in Eucommiae Cortex.

• International Journal of Molecular Medicine
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• 제44권5호
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• pp.1741-1752
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• 2019

In the present study, a polyphenolic mixture was isolated from Seomae mugwort (SM; a native Korean variety of Artemisia argyi H.) via extraction with aqueous 70% methanol followed by the elution of ethyl acetate over a silica gel column. Each polyphenolic compound was analyzed using high-performance liquid chromatography coupled with tandem mass spectrometry, and compared with the literature. In addition to the 14 characterized components, one hydroxycinnamate, six flavonoids, and one lignan were reported for the first time, to the best our knowledge, in Artemisia argyi H. The anti-inflammatory properties of SM polyphenols were studied in lipopolysaccharide-treated RAW 264.7 macrophage cells. The SM polyphenols attenuated the activation of macrophages via the inhibition of nitric oxide production, nuclear factor-κB activation, the mRNA expression of inducible nitric oxide synthase, tumor necrosis factor α and interleukin-1β, and the phosphorylation of mitogen-activated protein kinase. Our results suggested that SM polyphenols may have therapeutic potential for the treatment of inflammatory-related diseases.

• Journal of the korean society of oceanography
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• 제36권4호
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• pp.101-108
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• 2001

Polybrominated diphenylether (PBDEs) congeners, 2,4,4'-TrBDE, 2,2',4,4'-TeBDE, 2,2',4,4',5-PeBDE, 2,2',4,4',5,5'-HXBDE, and 2,2',4,4',5,6-HxBDE, were measured in sediments from 52 stations in the southeastern coastal areas of Korea. Sediment samples were analyzed using gas chromatography coupled to mass spectrometer detector (GC/MSD) with positive electron impact (PEI) mode. New analytical methodology for PBDEs by the isotope dilution method was established using a multi-layer silica gel column chromatography. Total PBDEs levels in sediments for Pohang coast ranged from 1,1 to 33.8 ng/g dry weight (mean 5.3 ng/g dry), from 1.6 to 36.4 ng/g dry weight (mean 5.7 ng/g dry) for Ulsan coast, from 0.8 to 20.3 ng/g dry weight (mean 4.9 ng/g dry) for Busan coast, and from 0.8 to 10.3 ng/g dry weight (mean 4.4 ng/g dry) for Jinhae Bay. PBDEs contamination in surface sediments from Korean southeastern coasts was relatively moderate in comparison to that of other marine environment in the world. The predominant PBDE congeners were 2,2',4,4'-TeBDE and 2,2',4,4',5-PeBDE.

• Journal of Pharmaceutical Investigation
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• 제41권5호
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• pp.309-315
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• 2011

A sensitive and specific liquid chromatographic method coupled with tandem mass spectrometry (LC-MS/MS) was developed for the analysis of ambroxol (active moiety of acebrophylline). After acetonitrile precipitation of proteins from plasma samples, ambroxol and the domperidone (internal standard, IS) were eluted on a C18 column. The isocratic mobile phase was consisted of 10 mM ammonium acetate and methanol (10 : 90, v/v), with flow rate at 0.2 mL/min. A tandem mass spectrometer, as detector, was used for quantitative analysis in positive mode by a multiple reaction monitoring mode to monitor the m/z 379.2${\rightarrow}$264.0 and the m/z 426.2${\rightarrow}$175.1 transitions for ambroxol and the IS, respectively. Twenty four healthy Korean male subjects received two capsules (100 mg ${\times}$ 2) of either the test or the reference formulation of acebrophylline HCl in a 2 ${\times}$ 2 crossover study, this was followed by a 1week washout period between either formulation. $AUC_{0-t}$ (the area under the plasma concentration-time curve) was calculated by the linear trapezoidal rule. $C_{max}$ (maximum plasma drug concentration) and $T_{max}$ (time to reach $C_{max}$) were compiled from the plasma concentration-time data. The 90% confidence intervals for the log transformed data were acceptable range of log 0.8 to log 1.25 (e.g., log 0.8964 - log 0.9910 for $AUC_{0-t}$ log 0.8690 - log 1.0750 for $C_{max}$). The major parameters, $AUC_{0-t}$ and $C_{max}$ met the criteria of Korea Food and Drug Administration for bioequivalence indicating that Acephyll$^{(R)}$ capsule (test) is bioequivalent to Surfolase$^{(R)}$ capsule (reference).

• Journal of Applied Biological Chemistry
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• 제50권4호
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• pp.244-248
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• 2007

The contents of total phenol and total flavonoid of artichoke (Cynara scolymus L.) were measured. The antioxidant activity of the artichoke was evaluated based on its potential as a scavenging the ABTS radical. These results showed the antioxidant activity of artichoke has a close relationship with the total flavonoid content. The compound showing antioxidant activity was isolated from the artichoke by repeated column chromatography and recrystallization. Based on the spectrometric studies, the compound was identified as 1,3-dicaffeoylquinic acid, known as cynarin. The content of cynarin from heads and leafs of the artichoke determined by $C_{18}$ reversed phase HPLC (high-performance liquid chromatography) coupled with photodiode array detector was 10.15 and 0.67 mg/g, respectively. This compound showed potent antioxidant activities against DPPH and ABTS radicals ($EC_{50}$ = 14.09 and 28.85 ${\mu}M$, respectively).

• 생약학회지
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• 제48권4호
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• pp.320-328
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• 2017

Yongdamsagan-tang has been used to treat the urinary disorders, acute- and chronic-urethritis, and cystitis in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was established for simultaneous analysis of the 20 bioactive marker compounds, geniposidic acid, chlorogenic acid, geniposide, liquiritin apioside, acteoside, calceolarioside B, liquiritin, nodakenin, baicalin, liquiritigenin, wogonoside, baicalein, glycyrrhizin, wogonin, glycyrrhizin, wogonin, saikosaponin A, decursin, decursinol angelate, alisol B, alisol B acetate, and pachymic acid in traditional herbal formula, Yongdamsagan-tang. Chromatographic separations of all marker compounds were conducted using a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) at $45^{\circ}C$ using a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. The MS analysis was performed using a Waters ACQUITY TQD LC-MS/MS coupled with an electrospray ionization source in the positive and negative modes. The flow rate was 0.3 mL/min and injection volume was $2.0{\mu}L$. The correlation coefficient of 20 marker compounds in the test ranges was 0.9943-1.0000. The limits of detection and quantification values of the all marker components were 0.11-6.66 and 0.34-19.99 ng/mL, respectively. As a result of the analysis using the optimized LC-ESI-MS/MS method, three compounds, geniposidic acid (from Plantaginis Semen), alisol B (from Alismatis Rhizoma), and pachymic acid (from Poria Sclerotium), were not detected in this sample. While the amounts of the 17 compounds except for the geniposidic acid, alisol B, and pachymic acid were $0.04-548.13{\mu}g/g$ in Yongdamsagan-tang sample. Among these compounds, baicalin, bioactive marker compound of Scutellariae Radix, was detected at the highest amount as a $548.13{\mu}g/g$.

• 생약학회지
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• 제47권1호
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• pp.92-101
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• 2016

In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was established for simultaneous determination of the 25 marker components, including chlorogenic acid, gallic acid, oxypaeoniflorin, homogentisic acid, methyl gallate, caffeic acid, 3,4-dihydroxybenzaldehyde, paeoniflorin, albiflorin, liquiritin, nodakenin, ferulic acid, ginsenoside Rg1, liquiritigenin, coumarin, cinnamic acid, benzoylpaeoniflorin, ginsenoside Rb1, cinnamaldehyde, paeonol, glycyrrhizin, 6-gingerol, evodiamine, rutecarpine, and spicatoside A in traditional Korean formula, Onkyung-tang. All analytes were separated on a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) at $45^{\circ}C$ using a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. The MS analysis was carried out using a Waters ACQUITY TQD LC-MS/MS coupled with an electrospray ionization (ESI) source in the positive and negative modes. The flow rate and injection volume were 0.3 mL/min and $2.0{\mu}L$, respectively. The correlation coefficient of all analytes in the test ranges was greater than 0.98. The limits of detection and quantification values of the 25 marker compounds were in the ranges 0.03-19.43 and 0.09-58.29 ng/mL, respectively. As a result, methyl gallate, 3,4-dihydroxybenzaldehyde, evodiamine, and rutecarpine were not detected in this sample and the concentrations of the 21 compounds except for the above 4 compounds were $33.09-3,496.32{\mu}g/g$ in Onkyung-tang decoction. Among these compounds, paeonol was detected at the highest amount as a $3,496.32{\mu}g/g$.