• Title/Summary/Keyword: microwave-assisted methodology

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Optimization of Microwave-Assisted Method for Accelerated Glycated Hemoglobin Quantification from Amino Acids to Proteins

  • Tran, Thi Thanh Huong;Jeong, Ji-Seon
    • Mass Spectrometry Letters
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    • v.8 no.3
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    • pp.53-58
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    • 2017
  • Glycated hemoglobin ($HbA_{1c}$) has been commonly used to screen and diagnose for patients with diabetes mellitus. Here the accelerated procedure of microwave-assisted sample treatment from acid hydrolysis to enzyme digestion followed by isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS) was optimized and applied to measure $HbA_{1c}$ in an effort to speed up analysis time. First, two signature peptides of $HbA_{1c}$ and hemoglobin $A_0$ were certified with amino acid analysis by setting optimized acid hydrolysis conditions to $150^{\circ}C$, 1.5 h and $10{\mu}M$ sample concentration in 8 M hydrochloric acid. Consequently, the accurate certified peptides above were used as calibration standards to implement the proteolytic procedure with endoproteinase Glu-C at $37^{\circ}C$, 700 W for 6 h. Compared to the traditional method, the microwave heating not only shortened dramatically sample preparation time, but also afforded comparable recovery yields. The optimized protocol and analytical conditions in this study are suitable for a primary reference method of $HbA_{1c}$ quantification with full SI-traceability and other similar proteins in complex biological samples.

Optimization of Microwave-Assisted Extraction under Atmospheric Pressure Condition for Soluble Ginseng Components (상압조건의 마이크로웨이브 추출공정에서 가용성 인삼성분의 추출조건 최적화)

  • Kwon, Joong-Ho;Kim, Kyung-Eun;Lee, Gee-Dong
    • Korean Journal of Food Science and Technology
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    • v.32 no.1
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    • pp.117-124
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    • 2000
  • Considering the thermal unstableness of ginseng components, microwave-assisted extraction(MAE) was performed under the atmospheric pressure condition. The monitoring of extraction characteristics and the optimization of extraction conditions were made by response surface methodology. The extraction efficiency of soluble ginseng components was high at lower ethanol concentration and at higher microwave power, while crude saponin content was easily extracted at higher ethanol concentration. Estimated conditions for the maximized extraction of soluble components including crude saponin, total phenolics and electron donating ability were $54{\sim}60%$ in ethanol concentration, $41{\sim}90$ W in microwave power, and within 4 min in extraction time. Predicted values at the optimum condition(60% ethanol, 80 W microwave power and 4 min extraction time) were in good agreement with observed values.

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Characteristics of Microwave-assisted Extraction for Catechins from Grape Seed (포도씨 카테킨류의 마이크로웨이브 추출특성)

  • Lee, Eun-Jin;Choi, Sang-Won;Kim, Hyun-Ku;Kwon, Joong-Ho
    • Korean Journal of Food Science and Technology
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    • v.40 no.5
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    • pp.510-515
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    • 2008
  • Microwave energy was applied to the extraction of functional catechins from grape seed. The solvent, absolute ethanol, reached the boiling point when exposed for less than 3 min microwave treatment at 100 W. The effects of independent variables in microwave-assisted extraction (MAE), including microwave power (0-160W, $X_1$), ethanol concentration (0-100%, $X_2$) and extraction time (1-5 min, $X_3$), were investigated on each response variable ($Y_n$), and the contents of catechin and its derivatives were determined via response surface methodology, thereby allowing us to predict their optimal extraction conditions. The predicted maximal values of (+)-catechin, procyanidin $B_2$, (-)-epicatechin, and (-)-epicatechin gallate were 137.99, 72.78, 222.38, and 9.59 mg%, respectively, under different MAE conditions. The predicted extraction conditions for maximum catechin responses were as follows: 104.10 W of microwave power, 45.35% of EtOH, and 4.89 min of extraction time for (+)-catechin (137.99 mg%), 133.16 W, 46.16% and 4.49 min for procyanidin $B_2$ (72.78 mg%), 136.00 W, 41.37% and 4.39 min for (-)-epicatechin (222.38 mg%), 143.20 W, 37.51% and 1.88 min for (-)-epicatechin gallate (9.59 mg%), respectively. The contents of (+)-catechin, procyanidin 1B2 and (-)-epicatechin in MAE were similarly influenced by three independent variables, whereas (-)-epicatechin gallate was influenced less profoundly by ethanol concentration and extraction time.

Prediction of Optimal Extraction Conditions in Microwave-Assisted Process for Antioxidant-Related Components from Thymus quinquecostatus (Microwave-Assisted Process에 의한 섬백리향의 항산화 관련 성분의 최적 추출조건 예측)

  • Kwon Young-ju;Noh Jung-eun;Lee Jung-eun;Lee Sung-Ho;Choi Yong-Hee;Kwon Joong-Ho
    • Food Science and Preservation
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    • v.12 no.4
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    • pp.344-349
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    • 2005
  • Microwave-assisted process (MAP) was applied to extract antioxidant-related components from Thymus quinquecostatus var. japonica Hara. Microwave power(2,450 MHz, $0{\sim}160$ W) and extraction time($1{\sim}5\;min$) were used as independent variables($X_i$) for central composite design to yield 10 different extraction conditions. Response surface methodology was applied to predict optimum extraction conditions for dependent variables of extracts, such as total yield, total phenolics, flavonoid, and electron donation ability depending on different powers and extraction times of MAP. Determination coefficients($R^2$) of regression equations for dependent variables were higher than 0.93 excluding that of total phenolics, and microwave power was predicted more influential than extraction time in MAP (p<0.05). The optimal extraction time for each dependent variable was ranged from 3.36 to 4.97 min, but microwave power showed wide ranges depending on variables. The superimposed contour maps for maximized dependent variables illustrated extraction conditions of 64 to 100 W in microwave power and 2.9 to 4.0 min in extraction time.

Monitoring of Extraction Properties of Ginseng Components during Pressurized Micorwave-Assisted Extraction (가압조건의 마이크로웨이브 추출에서 몇가지 인삼성분의 추출특성 모니터링)

  • 권중호;이새봄;이기동;정용진;김정숙
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.28 no.5
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    • pp.1087-1091
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    • 1999
  • Microwave extraction system equipped with closed vessels, which is known to rapidly extract target compounds from natural products, was applied to monitor the changes in phenolic compounds, browning color intensity and electron donating ability by using response surface methodology(RSM). Maximum content of phenolic compound was 21.65mg/100ml in 67.88% of ethanol concentration, 145oC of extraction temperature, and 6.24min of extraction time. The phenolic compounds in extracts are dependent on the increase of the extraction temperature and the ethanol concentration. Browning color intensity, which was maximized in 67.21%, 147oC, and 6.02min, was proportional to the increase of the extraction temperature. Maximum value of electron donating ability was 24.50units in 54.33%, 147oC, and 6.11 min. The electron donating ability of extracts was dependent on the increase of extraction temperature and maximized in the range from 50 to 65% of ethanol concentration.

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Optimization of Microwave-Assisted Pretreatment Conditions for Enzyme-free Hydrolysis of Lipid Extracted Microalgae (탈지미세조류의 무효소 당화를 위한 마이크로파 전처리 조건 최적화)

  • Jung, Hyun jin;Min, Bora;Kim, Seung Ki;Jo, Jae min;Kim, Jin Woo
    • Korean Chemical Engineering Research
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    • v.56 no.2
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    • pp.229-239
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    • 2018
  • The purpose of this study was to effectively produce the biosugar from cell wall of lipid extracted microalgae (LEA) by using microwave-assisted pretreatment without enzymatic hydrolysis process. Response surface methodology (RSM) was applied to optimization of microwave-assisted pretreatment conditions for the production of biosugar based on enzyme-free process from LEA. Microwave power (198~702 W), extraction time (39~241 sec), and sulfuric acid (0~1.0 mol) were used as independent variables for central composite design (CCD) in order to predict optimum pretreatment conditions. It was noted that the pretreatment variables that affect the production of glucose (C6) and xylose (C5) significantly have been identified as the microwave power and extraction time. Additionally, the increase in microwave power and time had led to an increase in biosugar production. The superimposed contour plot for maximizing dependent variables showed the maximum C6 (hexose) and C5 (pentose) yields of 92.7 and 74.5% were estimated by the predicted model under pretreatment condition of 700 w, 185.7 sec, and 0.48 mol, and the yields of C6 and C5 were confirmed as 94.2 and 71.8% by experimental validation, respectively. This study showed that microwave-assisted pretreatment under low temperature below $100^{\circ}C$ with short pretreatment time was verified to be an effective enzyme free pretreatment process for the production of biosugar from LEA compared to conventional pretreatment methods.

Prediction of the Optimum Conditions for Microwave-Assisted Extraction of the Total Phenolic Content and Antioxidative and Nitrite-scavenging Abilities of Grape Seed (포도씨의 총페놀 성분, 항산화능 및 아질산염소거능에 대한 마이크로웨이브 추출조건 예측)

  • Lee, Eun-Jin;Kim, Jeong-Sook;Kim, Hyun-Ku;Kwon, Joong-Ho
    • Food Science and Preservation
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    • v.18 no.4
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    • pp.546-551
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    • 2011
  • Response surface methodology (RSM) was used for the microwave-assisted extraction (MAE) of the effective components of grape seed, such as its antioxidative and nitrite-scavenging abilities. Microwave power (2,450 MHz, 0-160W), ethanol concentration (0-100%), and MAE time (1-5 min) were used as independent variables (Xi) for the central composite design to yield 16 different MAE conditions. The optimum MAE conditions were predicted for the dependent variables of the extracts, such as the total phenolic content ($Y_1$) antioxidative ability ($Y_2$), and nitrite-scavenging ability ($Y_3$), depending on different microwave powers, ethanol concentrations, and MAE times. The determination coefficients ($R^2$) of the regression equations for the dependent variables ranged from 0.8024 to 0.9498. The maximal values of each dependent variable were predicted at different MAE conditions, as follows: 3.19% total phenolic content at 142.32W, 44.30% ethanol, and 4.36 min, and 1.22 antioxidative ability at 84.44W, 56.60% ethanol, and 3.28 min. More than 99.5% nitrite-scavenging ability was predicted at pH 1.2-3.0, 30.80-106.58W, 49.32-55.18% ethanol, and 3.72-4.58min, respectively. The results indicated that the total phenolic content and anti oxidative ability showed a higher correlation with each other in that they were more influenced by microwave power than by the other variables, while the nitrite-scavenging ability was largely influenced by the ethanol concentration.

Monitoring of Extraction Characteristics and Comparison of Extraction Efficiencies for Ginsenosides in the Microwave-Assisted Process Under Pressure (가압조건의 마이크로웨이브 추출에서 Ginsenosides의 추출특성 모니터링과 추출효율 비교)

  • Lee Sae-Bom;Lee Gee-Dong;Kwon Joong-Ho
    • Journal of Ginseng Research
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    • v.23 no.3 s.55
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    • pp.164-171
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    • 1999
  • Microwave-assisted extraction, which is known to rapidly extract target compounds from natural products, was monitored by response surface methodology (RSM) while extracting ginsenosides by using microwave extraction system (MES) equipped with closed vessels, and was confirmed on its extraction efficiency. On the whole, coefficients of determinations $(R^2)$ of the models on ginsenoside contents of extracts with various extraction conditions were above 0.83 (p<0.1). $Ginsenoside-Rb_2,\;-Rc,\;-Re\;and\;-Rg_1$ were maximized in $140^{\circ}C$ of extraction temperature and $50\~75\%$ range of ethanol concentration. Unknown compound peak on HPLC chromatogram observed at extraction temperature over $120^{\circ}C$, increased at the extraction temperature of $150^{\circ}C$. The extraction temperature of $ginsenoside-Rb_2$ and -Re increased from $129^{\circ}C\;to\;147^{\circ}C$ with including unknown compound, and $R^2$ of the models on ginsenoside contents of extracts increased with including unknown compound into ginsenoside $Rb_2$ and Re. Contents of unknown compound were minimized in $67.33\%$ of ethanol concentration, $99.34^{\circ}C$ of extraction temperature and 3.65 min of extraction time. Ginsenoside contents extracted by microwave system for 8 min showed a similar tendency to those of the current extraction method for 40 hrs.

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Optimization of microwave-assisted extraction process for blue honeysuckle (Lonicera coerulea L.) using response surface methodology (반응표면분석법을 이용한 댕댕이 기능성성분의 마이크로웨이브추출조건 최적화)

  • Park, Daehee;Lee, Jae-Jun;Park, Jongjin;Park, Sanghwan;Lee, Wonyoung
    • Food Science and Preservation
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    • v.24 no.5
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    • pp.623-630
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    • 2017
  • Functional compounds including flavonoids, anthocyanins, polyphneols and antioxidants were extracted from blue honeysuckle (Lonicera caerulea L.) using highly efficient microwave-assisted extraction. And extraction process was modeled and optimized according to response surface methodology (RSM). The independent variables ($X_n$) were ethanol concentration ($X_1$: 0, 25, 50, 75, 100%), irradiation time ($X_2$: 1, 3, 5, 7, 9 min), and microwave power ($X_3$: 60, 120, 180, 240, 300 W). Dependent variables ($Y_n$) were total flavonoid contents ($Y_1$), total anthocyanin contents ($Y_2$), total polyphenol contents ($Y_3$) and antioxidant activity ($Y_4$). Four-dimensional response surface plots were generated based on the fitted second-order polynomial models to get optimal conditions. Estimated optimal conditions for 4 responses were ethanol concentration of 54-72%, irradiation time of 7.1-7.6 min, and microwave power of 243-251 W. Ridge analysis predicted the maximal responses of total flavonoid content, total anthocyanin content, total polyphenol content and antioxidant activity were 38.00 mg RE/g, 6.80 mg CGE/g, 14.90 mg GAE/g, 89.10%, respectively. Verification experiment was carried out at predicted optimal conditions and experimental values for total flavonoid content, total anthocyanin content, total polyphenol content and antioxidant activity were 38.10 mg RE/g, 6.72 mg CGE/g, 14.91 mg GAE/g and 89.13%, respectively. No significant difference was observed between predicted and experimental values, indicating good fitness of fitted model and successful application of RSM.

Base Catalysed Pyrimidine Synthesis Using Microwave

  • Kidwai, M.;Rastogi, S.;Saxena, S.
    • Bulletin of the Korean Chemical Society
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    • v.24 no.11
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    • pp.1575-1578
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    • 2003
  • An environmentally benign approach for the synthesis of 2-substituted-4,6-diaryl pyrimidines using inorganic solid supports for its catalytic role as well as an energy transfer medium is described. The methodology eliminates the usage of solvent during the reaction. The reaction time is brought down from hours to minutes along with yield enhancement. The rate enhancement and high yield is attributed to the coupling of solvent free conditions with microwaves. Further, the role of base is studied in the reaction and it is concluded that microwave assisted basic alumina catalysed reaction is the best in terms of catalysis as well as reaction time and yield.