• Title/Summary/Keyword: Liquid Liquid Extraction

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Development Rapid Analytical Methods for Inositol as a Trace Component by HPLC and LC-MS/MS in Infant Formula

  • Shin, Jin-Ho;Park, Jung-Min;Kim, Ha-Jung;Ahn, Jang-Hyuk;Kwak, Byung-Man;Kim, Jin-Man
    • Food Science of Animal Resources
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    • v.35 no.4
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    • pp.466-472
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    • 2015
  • A rapid and simple analytical method, using liquid chromatography tandem mass spectrometry (LC-MS/MS), was developed to detect myo-inositol (MI) in infant formulas. For protein removal: acid hydrolysis and lipid removal through organic solvent extraction. The operating conditions for instrumental analysis were determined based on previously reported analogous methods that used LC-MS/MS. Quantitative analysis was used for the detection limit test, infant formula recovery test, and standard reference material (SRM) 1849a to verify the validity of our LC-MS/MS analytical method, which was developed to quantify MI. For validation, the results of our method were compared with the results of quantitative analyses of certified values. The test results showed that the limit of detection was 0.05 mg/L, the limit of quantitation was 0.17 mg/L, and the method detection limit was 17 mg/kg. The recovery test exhibited a recovery between 98.07-98.43% and a relative standard deviation between 1.93-2.74%. Therefore, the result values were good. Additionally, SRM 1849a was measured to have an MI content of 401.84 mg/kg and recovery of 98.25%, which is comparable to the median certified value of 409 mg/kg. From the aforementioned results, we judged that the instrumental analysis conditions and preparation method used in this study were valid. The rapid analytical method developed herein could be implemented in many laboratories that seek to save time and labor.

Quantitative Determination of Ascaridole, Carvacrol and p-Cymene in the Biopesticides Products Derived from Chenopodium ambrosioides L. Extracts by Gas Chromatography

  • Yang, Ji-Yeon;Ryu, Song-Hee;Lim, Sung-Jin;Choi, Geun-Hyoung;Park, Byung-Jun
    • Korean Journal of Environmental Agriculture
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    • v.35 no.3
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    • pp.211-215
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    • 2016
  • BACKGROUND: The commercial biopesticides containing Chenopodium ambrosioides L. extracts which have been registered as one of the ingredients of the commercial biopesticide by the organic agriculture materials, and have been widely used in Republic of Korea. However, the quantitative analysis method of the active substances for the commercial biopesticides containing C. ambrosioides L. extract has not been conducted.METHODS AND RESULTS: To analyze the quantitative analysis of ascaridole, carvacrol, and p-cymene as active substances of C. ambrosioides L. extract, hydrophilic lipophilic balance cartridge was used for solid phase extraction. The active substances were analyzed by the gas chromatography with flame ionization detector. The limit of quantitation values of ascaridole, carvacrol, and p-cymene were 10, 5, and 2 mg/L, and the recovery rates were 96.3, 84.0, and 82.5% in liquid products and 98.3, 99.1, and 97.3% in solid products, respectively. The total content of ascaridole, carvacrol, and p-cymene in the commercial biopesticides was ranged from 0.08 to 12.75%.CONCLUSION: From these results, this method was suitable for the quantitative analysis of the active substances of commercial biopesticides containing C. ambrosioides L. extract.

Strength Characteristic and Color Difference Analysis of Cement Mortar According to the Amount of Liquefied Red Mud (액상화 레드머드의 첨가량에 따른 시멘트 모르타르의 강도특성 및 색차 분석)

  • Kang, Suk-Pyo;Kang, Hye-Ju
    • Journal of the Korean Recycled Construction Resources Institute
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    • v.6 no.2
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    • pp.146-152
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    • 2018
  • In the construction sector, new demands for aesthetics are increasing due to structural stability and improvement of living standard and consciousness level. On the other hand, Red Mud sludge is generated from aluminum hydroxide extraction process from Bauxite. Red mud sludge contains about 20% of $Fe_2O_3$ and represents a natural reddish brown. It is highly applicable to the construction industry. In this paper, red mud sludge with a water content of 50%, which is a by - product of the industry, was prepared as a liquid phase. The liquefied red mud was added to cement mortar and the strength and color difference of cement mortar were investigated according to the addition amount of liquefied red mud. As a result, the compressive strength decreased with increasing amount of liquefied red mud. The color of cement mortar containing liquefied red mud was found to be distributed in the range of YR series in all samples. As the amount of liquefied red mud increased, the color became darker.

Determination of 8-iso-PGF as Oxidative Stress Marker in Human Urine by High Performance Liquid Chromatography with Tandem Mass Spectrometry (LC/MS/MS를 이용한 산화성 스트레스 지표로써 소변 중 8-iso-PGF 분석)

  • Kho, Young-Lim;Lee, Eun-Hee;Chae, Hong-Jae;Choi, Kyung-Ho;Paik, Do-Myung
    • Journal of Environmental Health Sciences
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    • v.36 no.1
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    • pp.44-51
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    • 2010
  • This study aimed to develop analytical method for 8-isoprostanes as biomarkers for oxidative stress with LC/MS/MS technique and to apply the method for human urine samples. Analyzed compounds for urinary oxidative stress markers were 7 stereo-isomers of prostaglandins and the internal standard (iso-$PGF_{2{\alpha}}-d_4$) was used to adjust the recovery rate. The method for determining urinary iso-$PGF_{2{\alpha}}$ consisted of solid phase extraction and LC/MS/MS detection. Separation of isomers of prostaglandins completed by porous graphitic carbon column and buffer solution. Detection limits for urinary markers of oxidative stress, iso-$PGF_{2{\alpha}}$ with LC/MS/MS were 0.01 ng/ml by S/N ratio 3 and 0.028 ng/ml by calculated as to FDA method. The recovery (92.8~101.9%) and precision (8.8~20.7%) of analysis were feasible for detecting iso-$PGF_{2{\alpha}}$ in real human urine samples. We detected 4 isomers of prostaglandins in human urine samples. Mean (standard deviation) of urinary iso-$PGF_{2{\alpha}}$ concentration were 0.231 (0.117) ng/mg creatinine for smoking group and 0.154 (0.082) ng/mg creatinine for non-smoking group.

Identification and Quantitative Determination of Glucosinolates in Brassica napus cv. Hanakkori

  • Kim, Sun-Ju;Fujii, Kouei;Mohamed, Zaidul Islam Sarker;Kim, Hyun-Woong;Yamauchi, Hiroaki;Ishii, Gensho
    • Food Science and Biotechnology
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    • v.17 no.5
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    • pp.1097-1101
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    • 2008
  • The objective of this study was to identify and quantify glucosinolates (GSLs) in Brassica napus cv. Hanakkori and its parents and to evaluate its potential bitter taste. 'Hanakkori' materials were cultivated with commercial chemical nutrients (20 kg/ha, N-P-K: 16-10-10) at the field. GSLs were isolated by means of extraction with 70%(v/v) boiling methanol (MeOH) followed by desulfation from those plants by reversed-phase high performance liquid chromatography (HPLC) and identified by electronic spray ionization-mass spectrometry (ESI-MS) analysis. In 'Hanakkori', 11 GSLs were identified as progoitrin, glucoraphanin, glucoalyssin, gluconapoleiferin, gluconapin, 1-methylpropyl, glucobrassicanapin, glucobrassicin, 4-methoxyglucobrassicin, gluconasturtiin, and neoglucobrassicin. The total GSL contents were 109 and 36.1 mmol/kg dry weights (d.w.) for the seeds and edible parts, respectively. The major GSLs (>5 mmol/kg d.w.) in the seeds were progoitrin (78.8), gluconapin (10.7), and glucobrassicanapin (7.81), whereas they in the edible parts were progoitrin (16.1) and glucobrassicanapin (8.58). In addition, the bitter taste in the edible parts was presumably related with the presence of progoitrin (>45% to the total GSL).

Purification and Structural Analysis of Surfactin Produced by Endophytic Bacillus subtilis EBS05 and its Antagonistic Activity Against Rhizoctonia cerealis

  • Wen, Cai-Yi;Yin, Zhi-Gang;Wang, Kai-Xuan;Chen, Jian-Guang;Shen, Shun-Shan
    • The Plant Pathology Journal
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    • v.27 no.4
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    • pp.342-348
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    • 2011
  • Bacillus subtilis EBS05, an endophytic bacteria strain isolated from a medicinal plant Cinnamomum camphor, can produce antagonistic compounds that effectively inhibit plant pathogenic fungi. The greenhouse experiments showed that wheat sharp eyespot disease (WSED) was reduced by 91.2%, 88.2% and 43.0% after the treatment with fermentation broth, bacteria-free filter and a fungicide fludioxonil, respectively. The culture broth of strain EBS05 can more effectively control WSED than can fludioxonil. The fermentation broth and bacteria-free filter ability to suppress WSED was not significantly different, suggesting that an active secreted substance played a major role in controlling WSED. Separation and purification of the active compounds was carried out by serial processes, including hydrochloric acid (pH 2.0) treatment, methanol extraction and Sephadex LH-20 column chromatography, silica gel column chromatography and reverse-phase high-pressure liquid chromatography (HPLC), respectively. The purified compounds, one of active peaks in the HPLC spectrum, were obtained from the collection. Analysis of the chemical structures by time-of-flight mass spectrometry (TOF-MS) and electrospray ionization mass spectrometry/mass spectrometry (ESI-MS/MS) showed that the active substances produced by the endophytic bacteria EBS05 are mixture of the ${\beta}$-hydroxy-C12~C15-$Leu^7$ surfactin A isomers with 1035.65 Da, 1021.64 Da, 1007.63 Da and 993.65 Da molecular weights, respectively.

Degradation Kinetics of Three Veterinary Antibiotics in Composted and Stockpiled Manure

  • Kim, Sung-Chul;Yang, Jae-E.;Ok, Yong-Sik;Jung, Doug-Young;Carlson, Kenneth
    • Korean Journal of Soil Science and Fertilizer
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    • v.45 no.1
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    • pp.43-50
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    • 2012
  • Two typical animal waste management practices, composting and stockpiling, were evaluated for their effect on the degradation of three veterinary antibiotics (VAs), chlortetracycline (CTC), tylosin (TYL), and monensin (MNS). The VAs were applied to horse manure plots subject to composting or stockpiling, and core samples were collected over a period of time. Selected buffer solutions were used to extract the VAs and analysis for concentration was conducted with solid phase extraction (SPE) followed by high performance liquid chromatography tandem mass spectrometry (HPLC/MS/MS) technique. The VAs demonstrated rapid dissipation within ten days followed by a gradual decrease in concentration until the end of the experimental period (141 days). All three VAs degraded more rapidly in the composting samples than in the stockpiling samples, particularly between 20 and 60 days of the observation period. Degradation of the three VAs generally followed a first-order kinetic model, and a fitted model with a calculated rate constant was determined for each treatment. TYL in composting showed the fastest degradation, with a calculated rate constant of $0.91day^{-1}$; the slowest degradation was exhibited by MNS in stockpiling, with rate constant of $0.17day^{-1}$. Calculated correlation coefficients ranged from 0.89 to 0.96, indicating a strong correlation between measured concentrations and fitted values in this study. Although concentration of TYL in composting treatment showed below detection limit during the test period, this study suggests that composting can reduce animal waste contaminants prior to field application as fertilizer.

Comparative Analyses of Bioactive Constituents from Forsythia suspensa and Forsythia viridissima by HPLC-DAD

  • Won, Tae-Hyung;Liao, Lijuan;Lee, Seung-Ho;Son, Jong-Keun;Shin, Jong-Heon
    • Natural Product Sciences
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    • v.17 no.4
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    • pp.328-336
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    • 2011
  • A high-performance liquid chromatography (HPLC) with diode array detector (DAD) method was established for the discrimination of a folk medicine Forsythia suspensa and Forsythia viridissima. Five and three representative metabolites of the lignan and phenolic glycoside classes were selected for the analysis from F. suspensa and F. viridissima, respectively. The optimal chromatographic conditions were obtained on an ODS column (5 ${\mu}m$, $4.6{\times}250$ mm) with the column temperature at $40^{\circ}C$. The mobile phase was composed of methanol and 0.3% acetic acid using an isocratic elution with the flow rate 1 mL/min. Detection wavelength was set at 280 nm. All calibration curves showed good linear regression ($r^2$ > 0.996) within test ranges. Limits of detection (LOD) and limits of quantitation (LOQ) values were lower than 0.096 and 0.291 ${\mu}g/mL$, respectively. The developed method provided satisfactory precision and accuracy with overall intra-day and inter-day variations of 0.07-0.63% and 0.14-0.62%, respectively, and the overall recoveries of 97.79-102.46% for all of the compounds analyzed. In addition, effectiveness of diverse extraction methods was compared to each other for the development of standard analytical method. The verified method was successfully applied to the quantitative determination of representative metabolites in fifty-three commercial F. suspensa samples and fifteen commercial F. viridissima samples from diverse sources. The overall analytical results showed the unequivocal differences in bioactive constituents between F. suspensa and F. viridissima.

Concentration and Environmental Loading of Veterinary Antibiotics in Agricultural Irrigation Ditches

  • Kim, Sung-Chul;Chung, Doug Young;Kim, Kye Hoon;Lee, Ja Hyun;Kim, Hyo Kyung;Yang, Jae E.;Ok, Yong Sik;Almarwei, Yaser A.O.
    • Korean Journal of Soil Science and Fertilizer
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    • v.45 no.6
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    • pp.867-876
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    • 2012
  • The concentration of veterinary antibiotics in aqueous and sediment matrices was measured in agricultural irrigation ditches bordering several animal-feeding operations (AFOs) and then compared to its concentration in the watershed. Analytical determination in aqueous samples was based on solid phase extraction (SPE) and appropriate buffer solutions were used to extract residuals in sediment samples. Separation and detection of extracted veterinary antibiotics were performed with high performance liquid chromatograph tandem mass spectrometry (HPLC/MS/MS). In general, higher concentrations of antibiotic were observed in the aqueous phase of irrigation ditches, with the highest concentration of erythromycin hydrochloride (ETM-$H_2O$) of $0.53{\mu}g\;L^{-1}$, than in aqueous watershed samples. In contrast, higher concentrations were measured in river sediment than in irrigation ditch sediment with the highest concentration of oxytetracycline of $110.9{\mu}g\;kg^{-1}$. There was a high calculated correlation ( > 0.95) between precipitation and measured concentration in aqueous samples from the irrigation ditches for five of the ten targeted veterinary antibiotics, indicating that surface runoff could be an important transport mechanism of veterinary antibiotics from field to environment. Further, environmental loading calculation based on measured concentrations in aqueous samples and flow information clearly showed that irrigation ditches were 18 times greater than river. This result suggests the likelihood that veterinary antibiotics can be transported via irrigation ditches to the watershed. The transport via surface runoff and likely environmental loading via irrigation ditches examined in this study helps identify the pathway of veterinary antibiotics residuals in the environment.

Phenolic Profiles of Hardy Kiwifruits and Their Neuroprotective Effects on PC-12 and SH-SY5Y Cells against Oxidative Stress

  • Jeong, Ha-Ram;Kim, Kwan Joong;Lee, Sang Gil;Cho, Hye Sung;Cho, Youn-Sup;Kim, Dae-Ok
    • Journal of Microbiology and Biotechnology
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    • v.30 no.6
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    • pp.912-919
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    • 2020
  • Hardy kiwifruits (Actinidia arguta Planch.) have high amounts of antioxidants, including ascorbic acid (vitamin C) and phenolics. The anti-cholinesterase activity and neuroprotective effects of three different cultivars of hardy kiwifruits, cv. Mansu (A. arguta × A. deliciosa), cv. Haeyeon (A. arguta), and cv. Chiak (A. arguta), on PC-12 and SH-SY5Y cells were evaluated. Extraction of phenolics and vitamin C was carried out using 80% (v/v) aqueous ethanol and metaphosphoric acid assisted with homogenization, respectively. Hardy kiwifruit of cv. Mansu showed higher total phenolic, total flavonoid, and vitamin C contents and antioxidant capacity compared to the other two cultivars of hardy kiwifruits, cv. Haeyeon and cv. Chiak. Analysis of high-performance liquid chromatography results revealed the presence of procyanidin B2, (-)-epicatechin, neochlorogenic acid, cryptochlorogenic acid, rutin, hyperoside, isoquercitrin, and astragalin in hardy kiwifruits. The three cultivars of hardy kiwifruits had a wide range of vitamin C content of 55.2-130.0 mg/100 g fresh weight. All three cultivars of hardy kiwifruits had protective effects on neuronal PC-12 and SH-SY5Y cells exposed to hydrogen peroxide by increasing cell viability and reducing intracellular oxidative stress. Furthermore, the hardy kiwifruits inhibited acetylcholinesterase and butyrylcholinesterase. Collectively, these results suggest that hardy kiwifruits rich in antioxidants like phenolics and vitamin C have good potential as functional materials in neuroprotective applications.