• Title/Summary/Keyword: 6 M formic acid

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Component Analysis and Antioxidative Activity of Castanopsis cuspidata var. sieboldii Nut (구실잣밤나무 열매의 성분분석 및 항산화활성 평가)

  • Lee, Seung-Je;An, Ki-Wan;Choi, Tae-Soo;Jung, Hyeong-Seok;Moon, Jea-Hak;Park, Keun-Hyung
    • Food Science and Preservation
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    • v.17 no.1
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    • pp.139-144
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    • 2010
  • This study was carried out to investigate potential applications of the extract of Castanopsis cuspidata var. sieboldii $N_{AKAI}$ nut as a functional food ingredient. The pH and $^{\circ}Brix$ of nut were 6.43 and 3.17, respectively. L, a and b values as Hunter's color were 83.07, 1.49 and 10.48, respectively. Total content of monosaccharide was 54.26 mg% and organic acids were composed of oxalic acid 495.37 mg%, formic acid 200.03 mg%, malic acid 93.65 mg%, citric acid 27.80 mg%, and succinic acid 16.61 mg%. Total phenolic contents in various solvent extracts were as follows: water 27.69 mg%, 75% ethanol 16.50 mg%, ethyl acetate 16.50 mg%, and methanol 10.30 mg%. The antioxidant activity ($SC_{50},\;{\mu}g/mL$) of the nut extracts by various solvents was in the order of ethyl acetate 74.88 > methanol 155.00 > n-hexane 213.33 > ethanol 249.33 > butanol 274.78 > chloroform 314.67 > 75% ethanol 848.33 > water extracts 869.67. The results indicated that the extract of C. cuspidata nut contained a potential food ingredient.

Stability of Anthocyanin Pigment from Juice of Raspberries (나무딸기(복분자(覆盆子)) 과즙색소(果汁色素) Anthocyanin의 안정성(安定性)에 관한 연구(硏究))

  • Park, Jung-Mi;Joo, Kwang-Jee
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.11 no.3
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    • pp.67-74
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    • 1982
  • The effect of various pH levels, temperatures. organic acids, inorganic salts, metal ions on the stability of the anthocyanins pigment (pH 3.7) from the juice of raspberries were investigated. Initial absorption of total anthocyanin was decreased as pH increased from 1.0 to 7.0. Total amount of anthocyanin reached the highest at pH 3.7 and least at pH 7.0. The total anthocyanin content decreased rapidly with the increasing temperature. Many organic acids were found to enrich and stabilize the color density at 520nm in anthocyanin solution (pH 3.7). The hyperchromic effect of saturated n-carboxylic acid increased in the following order; formic acid> acetic acid>n-butyric acid>propionic acid. On the polycarboxylic acid, especially, malic acid showed 550$\sim$930% higher than control group. On the inorganic salts (0.5M), sodium perchlorate had the most hyperchromic effect and followed by sodium sulfate>sodium chloride>sodium phosphate, monobasic. Among the metal ions, both aluminium ion and cupric ion much more accelerated the anthocyanins degradation as compared with other metal ions.

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Recovery of Copper in Wastewater from Electroless Plating Process (무전해(無電解) 구리 도금폐액(鍍金廢液)으로부터 구리의 회수(回收) 연구(硏究))

  • Lee, Hwa Young;Ko, Hyun Baek
    • Resources Recycling
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    • v.21 no.6
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    • pp.39-44
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    • 2012
  • An attempt to recover copper from electroless plating wastewater has been made through evaporation followed by the electrowinning method. From the determination of each element in electroless plating wastewater, the content of Cu was found to be 582 mg/l and small amount of Fe was also contained in it. Moreover, the content of COD and TOC which was resulted from the addition of Rochell salt was found to be 9,560 and 13,100 mg/l, respectively. The content of formic acid generated by the oxidation of formaldehyde was determined to be 7.73 %. As a result, current efficiency was decreased with increase in current density and therefore current density less than $40mA/cm^2$ should be maintained to obtain current efficiency more than 80 %. The content of Fe in Cu obtained by electrowinning was found to be 0.021 and 0.01 % at the concentration of sulfuric acid of 2 and 10 vol%, respectively.

LC-MS Determination and Bioavailability Study of Imidapril Hydrochloride after the Oral Administration of Imidapril Tablets in Human Volunteers

  • Yun Ji Hye;Myung Ja Hye;Kim Hye Jin;Lee Sibeum;Park Jong-Sei;Kim Won;Lee Eun-Hee;Moon Cheol Jin;Hwang Sung-Joo
    • Archives of Pharmacal Research
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    • v.28 no.4
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    • pp.463-468
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    • 2005
  • The purpose of the present study was to develop a standard protocol for imidapril hydrochloride bioequivalence testing. For this reason, a specific LC-MS method was developed and validated for the determination of imidapril in human plasma. A solid-phase extraction cartridge, $Sep-pak^{R}$ C18, was used to extract imidapril and ramipril (an internal standard) from deproteinized plasma. The compounds were separated using a XTerra $MS^{R}$?C18 column ($3.5 {\mu}m, 2.1\times150 mm$) and $acetonitrile-0.1\%$ formic acid (67:33, v/v) adjusted to pH 2.4 by 2 mmol/L ammonium formic acid, as mobile phase at 0.3 mL/min. Imidapril was detected as m/z 406 at a retention time of ca. 2.3 min, and ramipril as m/z 417 at ca. 3.6 min. The described method showed acceptable specificity, linearity from 0.5 to 100 ng/mL, precision (expressed as a relative standard deviation of less than $15\%$), accuracy, and stability. The plasma concentration-versus-time curves of eight healthy male volunteers administered a single dose of imidapril (10 mg), gave an $AUC_{12hr}$ of imidapril of $121.48\pm35.81 ng mL^{-1} h$, and $C_{max} and T_{max}$ values of $32.59\pm9.76 ng/mL and 1.75\pm0.27 h$. The developed method should be useful for the determination of imidapril in plasma with sufficient sensitivity and specificity in bioequivalence study.

Simultaneous Determination of Baicalein, Baicalin, Wogonin, and Wogonoside in Rat Plasma by LC-MS/MS for Studying the Pharmacokinetics of the Standardized Extract of Scutellariae Radix

  • Chung, Hye-Jin;Lim, Sun-Young;Kim, In-Sook;Bu, Young-Min;Kim, Ho-Cheol;Kim, Dong-Hyun;Yoo, Hye-Hyun
    • Bulletin of the Korean Chemical Society
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    • v.33 no.1
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    • pp.177-182
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    • 2012
  • A new composition of standardized Scutellariae Radix extract (HPO12) was developed for treatment of Alzheimer's disease. For the preclinical pharmacokinetic study of HPO12, a rapid, sensitive, and selective LCMS/MS method was developed and validated for the simultaneous determination of 4 bioactive compounds, baicalein, baicalin, wogonin, and wogonoside. After extraction with ethylacetate, chromatographic analysis was performed on a Thermo $C_{18}$ column ($150mm{\times}2.1mm$, $3{\mu}m$) with a mobile phase consisting of 0.1% formic acid (A) and 0.1% formic acid in 95% acetonitrile (B) by using gradient elution at a flow rate of $250{\mu}L/min$. Analytes introduced to a mass spectrometer were monitored by multiple reaction monitoring (MRM) in positive ion mode. Using $25{\mu}L$ of plasma sample, the method was validated over the following concentration ranges: 25-5000 ng/mL for baicalein, 20-40000 ng/mL for baicalin, 1-1000 ng/mL for wogonin, and 5-10000 ng/mL for wogonoside. The intra- and inter-day precision and accuracy of the quality control samples at the 4 concentrations showed $\leq$ 13.7% relative standard deviation (RSD) and 86.6-105.5% accuracy. The method was successfully applied to determine the concentrations of baicalein, baicalin, wogonin, and wogonoside in rat plasma after intraperitoneal and oral administrations of HPO12.

Simultaneous Analysis of Bioactive Metabolites from Lonicera japonica Flower Buds by HPLC-DAD-MS/MS (HPLC-DAD-MS/MS를 이용한 금은화 생리활성 물질의 동시분석)

  • Ryu, Sung-Kwang;Jeon, Ju-Eun;Kang, Gyoung-Won;Kang, Sam-Sik;Shin, Jong-Heon
    • YAKHAK HOEJI
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    • v.52 no.6
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    • pp.446-451
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    • 2008
  • A high-performance liquid chromatography (HPLC) with diode array detector (DAD) and electrospray ionization mass spectrometry (ESI-MS) was established for the simultaneous determination of chlorogenic acid (1), sweroside (2), luteolin-7-O-glucoside (3), (E)-aldosecologanin (4) and 3,5-dicaffeoylquinic acid (5) from Lonicera joponica flower buds. The optimal chromatographic conditions were obtained on an ODS column (5 ${\mu}m$, 4.6${\times}$150 mm) with the column temperature $25^{\circ}C$. The mobile phase was composed of (A) water with 0.1% formic acid and (B) acetonitrile with 0.1% formic acid using a gradient elution, the flow rate was 0.3 ml/min. Detection wavelength was set at 250 nm. All calibration curves showed good linear regression ($r^2$>0.994) within test ranges. The developed method provided satisfactory precision and accuracy with overall intra-day and inter-day variations of 0.05${\sim}$1.95% and 0.15${\sim}$2.26%, respectively, and the overall recoveries of 97.71${\sim}$103.65% for the five compounds analyzed. The verified method was successfully applied to quantitative determination of the three types (phenolic compounds, iridoids and flavonoids) of bioactive compounds in 21 commercial L. japonica flower buds samples from different markets in Korea and China. The analytical results demonstrated that the contents of the five analytes vary significantly with sources.

Quantitative Analysis of Eleven Bioactive Constituents of a Traditional Herbal Medicine, Yeonggyechulgam-tang using, Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Natural Product Sciences
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    • v.23 no.2
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    • pp.84-91
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    • 2017
  • This study proposes a sensitive and selective liquid chromatography-electrospray ionization tandem mass spectrometry method of efficiently assessing the quality of a traditional herbal medicine called Yeonggyechulgam-tang (YGCGT). The following compounds 1 - 11, namely, liquiritin apioside (1), liquiritin (2), liquiritigene (3), coumarin (4), cinnamic acid (5), cinnamaldehyde (6), glycyrrhizin (7), atractylenolide III (8), atractylenolide II (9), atractylenolide I (10), and pachymic acid (11) were separated on a UPLC BEH $C_{18}$ column ($2.1{\times}100mm$, $1.7{\mu}m$) at a column temperature of $45^{\circ}C$ eluted with a gradient condition of 0.1% (v/v) formic acid in distilled water and acetonitrile. The correlation coefficient of the calibration curve of the eleven constituents was ${\geq}0.9936$. The limits of detection and quantification of the compounds 1 - 11 were 0.06 - 4.73 ng/mL and 0.17-14.20 ng/mL, respectively. Using this analytical method, the compound 11 in lyophilized YGCGT decoction extract was not detected, while the compounds 1 - 10 were detected 0.13-166.43 mg/g.

Determination of Rosmarinic Acid and Caffeic Acid from Perilla frutescens var. japonica and var. acuta by Reversed-Phase HPLC (RP-HPLC를 이용한 백소엽(白蘇葉)과 자소엽(紫蘇葉)의 카페익산과 로즈마린산 분석)

  • Kim, Byung-Youn;Jeong, Ji-Seon;Kwon, Ha-Jeong;Lee, Je-Hyun;Hong, Seon-Pyo
    • The Korea Journal of Herbology
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    • v.23 no.3
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    • pp.67-72
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    • 2008
  • Objectives : This study presents a high performance liquid chromatography methods for the quantitative and qualitative analysis of rosmarinic acid (RA) and caffeic acid (CA) in Perilla frutescens var. japonica and var. acuta. Methods : Chromatographic separation was performed using a mixture of methanol, water and formic acid (35 : 64.2 : 0.8) with a reversed-phase column (Gemini C18, 4.6 ${\times}$ 150 mm, 3 ${\mu}m$). The analyses were detected at UV (280 nm). Results : The samples were extracted with 50% EtOH under reflux for 1 h, and simultaneous determination for RA and CA in hyang-so-san and haeng-so-san was possible without interference peaks Conclusions : According the results, we developed a determination method for RA and CA in Perillae Folium. Owing to Perilla frutescens var. japonica and var. acuta did not show significant difference in contents of RA and CA, both Perilla frutescens could be available as herbal medicine.

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Simultaneous Quantitative Determination of Nine Hallucinogenic NBOMe Derivatives in Human Plasma Using Liquid Chromatography Tandem Mass Spectrometry

  • Seo, Hyewon;Yoo, Hye Hyun;Kim, Young-Hoon;Hong, Jin;Sheen, Yhun Yhong
    • Mass Spectrometry Letters
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    • v.10 no.1
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    • pp.18-26
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    • 2019
  • We developed a bioanalytical method for simultaneous determination of nine NBOMe derivatives (25H-NBOMe, 25B-NBOMe, 25E-NBOMe, 25N-NBOMe, 25C-NBOH, 25I-NBOH, 25B-NBF, 25C-NBF, and 25I-NBF) in human plasma using liquid chromatography tandem mass spectrometry (LC-MS/MS). Human plasma samples were pre-treated using solid-phase extraction. Separation was achieved on a C18 column under gradient elution using a mobile phase containing 0.1% formic acid in acetonitrile and 0.1% formic acid in water at a flow rate of 0.3 mL/min. Mass detection was performed in the positive ion mode using multiple reaction monitoring. The calibration range was 1-100 ng/mL for all quantitative analytes, with a correlation coefficient greater than 0.99. The intra- and inter-day precision and accuracy varied from 0.85 to 6.92% and from 90.19 to 108.69%, respectively. The recovery ranged from 86.36 to 118.52%, and the matrix effects ranged from 27.09 to 99.72%. The stability was acceptable in various conditions. The LC-MS/MS method was validated for linearity, accuracy, precision, matrix effects, recovery and stability in accordance with the FDA guidance. The proposed method is suitable for reliable and robust routine screening and analysis of nine NBOMe derivatives in forensic field.

Development and Validation of a Liquid Chromatography-Tandem Mass Spectrometry Method for the Determination of ε-Acetamidocaproic Acid in Rat Plasma

  • Kim, Tae Hyun;Choi, Yong Seok;Choi, Young Hee;Kim, Yoon Gyoon
    • Toxicological Research
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    • v.29 no.3
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    • pp.203-209
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    • 2013
  • A simple and rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantification of ${\varepsilon}$-acetamidocaproic acid (AACA), the primary metabolite of zinc acexamate (ZAC), in rat plasma by using normetanephrine as an internal standard. Sample preparation involved protein precipitation using methanol. Separation was achieved on a Gemini-NX $C_{18}$ column ($150mm{\times}2.0mm$, i.d., 3 ${\mu}m$ particle size) using a mixture of 0.1% formic acid-water : acetonitrile (80 : 20, v/v) as the mobile phase at a flow rate of 200 ${\mu}l/min$. Quantification was performed on a triple quadrupole mass spectrometer employing electrospray ionization and operating in multiple reaction monitoring (MRM) and positive ion mode. The total chromatographic run time was 4.0 min, and the calibration curves of AACA were linear over the concentration range of 20~5000 ng/ml in rat plasma. The coefficient of variation and relative error at four QC levels were ranged from 1.0% to 5.8% and from -8.4% to 6.6%, respectively. The present method was successfully applied for estimating the pharmacokinetic parameters of AACA following intravenous or oral administration of ZAC to rats.