1.Simultaneous Determination of 11 Marker Compounds in Gumiganghwal-tang by HPLC-DAD and LC-MS.
Jin Bae WEON ; Youn Sik JUNG ; Gahee RYU ; Woo Seung YANG ; Choong Je MA
Natural Product Sciences 2016;22(4):238-245
Gumiganghwal-tang has been used for the treatment of common cold for a long-time. We developed an accurate and sensitive high performance liquid chromatography-diode array detection (HPLC-DAD) and electrospray ionization mass spectrometry method for the simultaneous determination of ferulic acid, baicalin, bergapten, methyl eugenol, glycyrrhizin, oxypeucedanin, wogonin, nodakenin, atractylenolide III, imperatorin, and atractylenolide I in Gumiganghwal-tang samples. The analytes were separated on a Shiseido C18 column (5 µm, 4.6 mm I.D. × 250 mm) with gradient elution with acetonitrile and 0.1% trifluoroacetic acid. Eleven compounds were quantitatively determined by HPLC-DAD and identified by LC-MS data. We also validated this method. The calibration curves of all the compounds showed good linear regression. The limits of detection and the limits of quantification ranged from 0.04 to 0.63 and from 0.12 to 1.92 µg/mL, respectively. The relative standard deviation values of intra- and inter-days of this method represented less than 2.9%. The recoveries were found to be in the range of 90.06 – 107.66%. The developed method has been successfully applied to the analysis of Gumiganghwal-tang samples. The established HPLC method could be used to quality control of Gumiganghwal-tang.
Calibration
;
Chromatography, High Pressure Liquid
;
Common Cold
;
Eugenol
;
Glycyrrhizic Acid
;
Limit of Detection
;
Linear Models
;
Methods
;
Quality Control
;
Spectrometry, Mass, Electrospray Ionization
;
Trifluoroacetic Acid
2.Phytochemical Analysis of the Phenolic Fat-Suppressing Substances in the Leaves of Lactuca raddeana in 3T3-L1 Adipocytes.
Agung NUGROHO ; Jae Sue CHOI ; Hyo Jin AN ; Hee Juhn PARK
Natural Product Sciences 2015;21(1):42-48
Lactuca raddeana (Compositae) is used to treat obesity and complications due to diabetes. The five phenolic compounds including chlorogenic acid, chicoric acid, luteolin 7-O-glucoside, luteolin 7-O-glucuronide, luteolin were qualitatively identified by LC-ESI-MS analysis. The contents were quantitatively determined by HPLC, under the condition of a Capcell Pak C18 column (5 microm, 250 mm x 4.6 mm i.d.) and a gradient elution of 0.05% trifluoroacetic acid (TFA) and 0.05% TFA in MeOH-H2O (60 : 40). The contents of chicoric acid (100.99 mg/g extract) and luteolin 7-O-glucoside (101. 69 mg/g extract) were high, while those of other three phenolic substances were very low. The 3T3-L1 adipocyte cells treated with chicoric acid and luteolin 7-O-glucuronide significantly suppressed the accumulation of fat, suggesting they are effective against obesity. Since high level of peroxynitrite (ONOO) causes cardiovascular disease in obese patients, its scavenging activity was also studied.
Adipocytes*
;
Asteraceae
;
Cardiovascular Diseases
;
Chlorogenic Acid
;
Chromatography, High Pressure Liquid
;
Humans
;
Luteolin
;
Obesity
;
Peroxynitrous Acid
;
Phenol*
;
Trifluoroacetic Acid
3.Rapid Isolation of Cyanidin 3-Glucoside and Peonidin 3-Glucoside from Black Rice (Oryza sativa) Using High-Performance Countercurrent Chromatography and Reversed-Phase Column Chromatography.
Heejin JEON ; Janggyoo CHOI ; Soo Jung CHOI ; Chang Uk LEE ; Shin Hee YOON ; Jinwoong KIM ; Kee Dong YOON
Natural Product Sciences 2015;21(1):30-33
Anthocyanins are water soluble plant pigments which are responsible for the blue, red, pink, violet colors in several plant organs such as flowers, fruits, leaves and roots. In recent years, anthocyanin-rich foods have been favored as dietary supplements and health care products due to diverse biological activities of anthocyanins including antioxidant, anti-allergic, anti-diabetic, anti-microbial, anti-cancer and preventing cardiovascular disease. High-performance countercurrent chromatography (HPCCC) coupled with reversed-phase medium pressure liquid chromatography (RP MPLC) method was applied for the rapid and efficient isolation of cyanidin 3-glucoside (C3G) and peonidin 3-glucoside (P3G) from black rice (Oryza sativa L., Poaceae). The crude black rice extract (500 mg) was subjected to HPCCC using two-phase solvent system composed of tert-butyl methyl ether/n-butanol/acetonitrile/0.01% trifluoroacetic acid (TBME/B/A/0.01% TFA, 1 : 3 : 1 : 5, v/v, flow rate - 4.5 mL/min, reversed phase mode) to give enriched anthocyanin extract (37.4 mg), and enriched anthocyanin extract was sequentially chromatographed on RP-MPLC to yield C3G (16.5 mg) and P3G (8.7 mg). The recovery rate and purity of isolated C3G were 76.0% and 98.2%, respectively, and those of P3G were 58.3% and 96.3%, respectively. The present study indicates that HPCCC coupled with RP-MPLC method is more rapid and efficient than multi-step conventional column chromatography for the separation of anthocyanins.
Anthocyanins
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Cardiovascular Diseases
;
Chromatography*
;
Chromatography, Liquid
;
Countercurrent Distribution*
;
Delivery of Health Care
;
Dietary Supplements
;
Flowers
;
Fruit
;
Plants
;
Trifluoroacetic Acid
;
Viola
4.Qualitative and quantitative analysis of fluoxetine hydrochloride by 19F NMR.
Bai-Qin YANG ; Er-Li KONG ; Xiao-Di XUE ; Shou-Qian ZHAO ; Shrong-Shi LIN
Acta Pharmaceutica Sinica 2012;47(5):630-633
The chemical shift of fluoxetine hydrochloride appears at delta 14.15 in 19F NMR analysis. The delta moved upfield slightly from 14.158 to 14.145 when the concentration of solution became diluted from 2.00 to 0.05 mmol x L(-1). Spiking test was suggested to confirm the existence of the compound for qualitative analysis. 19F NMR detection sensitivity test illustrated that a concentration of 17 mg in 1 L water could be detected while the sample was scanned 500 times with optimum parameters. In quantitative analysis, standard curve of concentration versus fluorine signal intensity was proposed to determine the amount of fluoxetine. Long capillary tube containing trifluoroacetic acid was used as internal standard for the integration measurements and straight line was obtained with good fitting. Direct additions of trifluoroethanol to fluoxetine solutions gave a poorer standard curve.
Fluorine
;
chemistry
;
Fluoxetine
;
analysis
;
chemistry
;
Magnetic Resonance Spectroscopy
;
Molecular Structure
;
Trifluoroacetic Acid
;
analysis
5.A Case of Chemical Burn Caused by Trifluoroacetic Anhydride that Mimicked a Hydrofluoric Acid Burn.
Jung Soo PARK ; Hoon KIM ; Suk Woo LEE
Journal of The Korean Society of Clinical Toxicology 2010;8(1):43-45
A 22-year-old woman was referred to our emergency department for the treatment of a chemical injury on her arm. She had accidentally spilled 99% trifluoroacetic anhydride (TFAA) over her left forearm during an organic chemistry experiment. She visited a primary care unit, and then she was referred to our hospital for inactivation of the released fluoride ions. Her skin lesions were different from those caused by hydrofluoric acid (HF) injury. The injured area showed painful whitish maculae and patchy areas with accentuated rim. No vesiculation and bulla formation was detected. We intradermally injected a 5% solution of calcium through a 24-gauge needle into the burned skin. After the injection, she complained of more severe pain. Although TFAA contains fluorine, it does not release free fluoride ions on contact with the skin, unlike HF. In fact, application of calcium gluconate for TFAA burns is not recommended. Rather, it should be avoided since it increases pain and local abscess formation.
Abscess
;
Acetic Anhydrides
;
Arm
;
Blister
;
Burns
;
Burns, Chemical
;
Calcium
;
Calcium Gluconate
;
Chemistry, Organic
;
Emergencies
;
Female
;
Fluorides
;
Fluorine
;
Fluoroacetates
;
Forearm
;
Gluconates
;
Humans
;
Hydrofluoric Acid
;
Ions
;
Needles
;
Primary Health Care
;
Skin
;
Trifluoroacetic Acid
;
Young Adult
6.Application of reversed-phase ion-pair chromatography for universal estimation of octanol-water partition coefficients of acid, basic and amphoteric drugs.
Hui ZHU ; Ri-Fang YANG ; Liu-Hong YUN ; Yu JIANG ; Jin LI
Acta Pharmaceutica Sinica 2009;44(9):1025-1028
This paper is to establish a reversed-phase ion-pair chromatography (RP-IPC) method for universal estimation of the octanol/water partition coefficients (logP) of a wide range of structurally diverse compounds including acidic, basic, neutral and amphoteric species. The retention factors corresponding to 100% water (logk(w)) were derived from the linear part of the logk'/phi relationship, using at least four isocratic logk' values containing different organic compositions. The logk(w) parameters obtained were close to the corresponding logP values obtained with the standard "shake flask" methods. The mean deviation for test drugs is 0.31. RP-IPC with trifluoroacetic acid as non classic ion-pair agents can be applicable to determine the logP values for a variety of drug-like molecules with increased accuracy.
1-Octanol
;
chemistry
;
Chromatography, Reverse-Phase
;
methods
;
Hydrogen-Ion Concentration
;
Octanols
;
chemistry
;
Trifluoroacetic Acid
;
Water
;
chemistry
7.A Successful Treatment of Patient with Fatal Complications after beta-fluoroethyl acetate Ingestion.
Journal of the Korean Society of Emergency Medicine 2008;19(5):588-594
The highly toxic sodium monofluoroacetate (SMFA) was banned as a rodenticide in this country in the 1980s. The fluoroacetate metabolite, fluorocitric acid blocks cellular metabolism by inhibiting the Klebs cycle, producing wide spread clinical effects including respiratory, neurologic, cardiologic, and fluid-electrolyte abnormalities. We report the survival case by continuous renal replacement therapy from fatal complications after beta-fluoroethyl acetate ingestion. 61-year old male was brought to our emergency center with chief complaint of beta-fluoroethyl acetate ingestion. Soon after 80 minutes of hospital admission, he developed the symptoms of mild metabolic acidosis, respiratory failure, coma, transient tachycardia, and refractory hypotension. On the second hospital day, we guessed that drug induced severe rhabdomyolysis and renal failure were in progress. At 28 hours after hospital admission, we started the continuous renal replacement therapy (CRRT) with the informed consent. Dramatically, at 24 hour after beginning the CRRT, the patient were completely recovered from coma, respiratory failure, and refractory shock, although severe rhabdomyolysis and renal failure still existed. Additionally, four times of hemodialysis were performed. On 25th hospital admission, he discharged with non oliguric renal failure state, arranging to return to out patient department.
Acidosis
;
Coma
;
Eating
;
Emergencies
;
Fluoroacetates
;
Humans
;
Hypotension
;
Informed Consent
;
Male
;
Renal Dialysis
;
Renal Insufficiency
;
Renal Replacement Therapy
;
Respiratory Insufficiency
;
Rhabdomyolysis
;
Rodenticides
;
Shock
;
Sodium
;
Tachycardia
8.Breeding of monofluoroacetate-resistant strains of Actinobacillus succinogenes and the mechanism based on metabolic flux analysis.
Yupeng LIU ; Pu ZHENG ; Ye NI ; Jinjun DONG ; Ping WEI ; Zhihao SUN
Chinese Journal of Biotechnology 2008;24(3):460-467
Succinic acid has received a great deal of attention as an important green chemical stock for the manufacture of synthetic resins, biodegradable polymers and chemical intermediates. In this paper, the breeding mechanism of Actinobacillus succinogenes based on metabolic flux analysis was demonstrated to improve the yield of succinic acid by fermentation. After the NTG treatment, mutants from A. succinogenes CGMCC 1593 which were able to grow in medium containing concentrations of about 50-100 mmol/L of sodium monofluoroacetate were obtained. Among them, a mutant SF-9 was selected for producing more succinic acid and less acetic acid. When fermentations were conducted in a 5 L bioreactors, the final succinic acid concentration of SF-9 (34.8 g/L) increased 23.4%, and the mass ratio of succinic acid/acetic acid increased from 3.3 to 9 compared with those of the parent strain. Based on the metabolic flux analysis of A. succinogenes, PEP was found to be a key node which has an important effect on the production of succinic acid, and the flux ratio of by-productions (acetic, formic, lactic acid) was influenced by PYR node. Compared with the parent strain, the flux to succinic acid of mutant (A. succinogenes SF-9) was significantly increased, while the flux to by-productions had an obvious decline. Therefore, PEP and PYR are not rigid nodes in the metabolic regulation of A. succinogenes.
Actinobacillus
;
genetics
;
growth & development
;
metabolism
;
Drug Tolerance
;
Fermentation
;
Fluoroacetates
;
metabolism
;
Metabolic Networks and Pathways
;
Mutation
;
Succinic Acid
;
metabolism

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