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Identification of Flavonoids from Extracts of Opuntia ficus-indica var. saboten and Content Determination of Marker Components Using HPLC-PDA (손바닥선인장 추출물의 플라보노이드 구조 규명 및 HPLC-PDA를 이용한 지표성분의 함량 분석)

  • Park, Seungbae;Kang, Dong Hyeon;Jin, Changbae;Kim, Hyoung Ja
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.46 no.2
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    • pp.210-219
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    • 2017
  • This study aimed to establish an optimal extraction process and high-performance liquid chromatography (HPLC)-photodiode array (PDA) analytical method for determination of marker compounds, dihydrokaempferol (DHK) and 3-O-methylquercetin (3-MeQ), as a part of materials standardization for the development of health functional foods from stems of Opuntia ficus-indica var. saboten (OFS). The quantitative determination method of marker compounds was optimized by HPLC analysis, and the correlation coefficient for the calibration curve showed very good linearity. The HPLC-PDA method was applied successfully to quantification of marker compounds in OFS after validation of the method in terms of linearity, accuracy, and precision. Ethanolic extracts from stems of O. ficus-indica var. saboten (OFSEs) were evaluated by reflux extraction at 70 and $80^{\circ}C$ with 50, 70, and 80% ethanol for 3, 4, 5, and 6 h. Among OFSEs, OFS70E at $80^{\circ}C$ showed the highest contents of DHK and 3-MeQ of $26.42{\pm}0.65$ and $3.88{\pm}0.29mg/OFS100g$, respectively. Furthermore, OFSEs were determined for their antioxidant activities by measuring 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging and lipid peroxidation (LPO) inhibitory activities in rat liver homogenate. OFS70E at $70^{\circ}C$ showed the most potent antioxidant activities with $IC_{50}$ values of $1.19{\pm}0.11$ and $0.89{\pm}0.09mg/mL$ in the DPPH radical scavenging and LPO inhibitory assays, respectively. To identify active components of OFS, various chromatographic separation of OFS70E led to isolation of 11 flavonoids: dihydrokaempferol, dihydroquercetin, 3-O-methylquercetin, quercetin, isorhamnetin 3-O-glucoside, isorhamnetin 3-O-galactoside, narcissin, kaempferol 7-O-glucoside, quercetin 3-O-galactoside, isorhamnetin, and kaempferol 3-O-rutinoside. The results suggest that standardization of DHK in OFSEs using HPLC-PDA analysis would be an acceptable method for the development of health functional foods.

Vitamin C Quantification of Korean Momordica charantia by Cultivar, Harvest Time, and Maturity (국내산 여주의 지역별, 수확시기별, 숙기별 Vitamin C 함량)

  • Jeong, Yun Sook;Lee, Sang Hoon;Song, Jin;Hwang, Kyung-A;Noh, Geon Min;Hwang, In Guk
    • The Korean Journal of Food And Nutrition
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    • v.29 no.4
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    • pp.474-479
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    • 2016
  • This study aimed to investigate the concentration of vitamin C in Momordica charantia (MC) by cultivar, harvest time, and maturity. The methods for determining vitamin C levels were validated by measuring their linearity, specificity, limit of detection (LOD), limit of quantification (LOQ), precision, and accuracy using HPLC. Results showed high linearity in the calibration curve, with a coefficient of correlation ($R^2$) of 0.9994. The LOD and LOQ values for vitamin C were 0.05 and $0.16{\mu}g/mL$, respectively. The relative standard deviations (RSDs) for intra- and inter-day precision of vitamin C measurements were 2.34 and 1.34%, respectively. Depending on cultivar, the concentration of vitamin C in MC varied from 20.75~107.31 mg/100 g, fresh weight, with an average level $68.85{\pm}25.57mg/100g$, FW. When MC was analyzed by harvest time, the 20150612 MC showed the highest amount of vitamin C ($113.20{\pm}1.89mg/100g$, FW). On the other hand, the highest vitamin C content by maturity was $48.59{\pm}0.87mg/100g$, FW (15 day old MC). This information on the comparative vitamin C levels of MC might be useful to food scientists and should be explored for functional food development.

Development of a Method for Analyzing the Nicotine Content in Synthetic Flavoring Substances as Unauthorized E-cigarette Liquid by Using HPLC (전자담배 액상 충진제와 유사한 합성착향료 중 니코틴의 HPLC 분석법 개발)

  • Kim, Jae-Young;Lee, Sang-Mok;Chang, Moon-Ik;Cho, Yoon-Jae;Lee, Han-Jin;Chae, Young-Sik;Rhee, Gyu-Sik
    • Korean Journal of Food Science and Technology
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    • v.45 no.6
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    • pp.693-699
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    • 2013
  • A simple, sensitive, and specific method for quantifying the nicotine content of synthetic favoring substances (SFS) was developed using high performance liquid chromatography (HPLC) with a photo-diode array detector (PDA). Nicotine was extracted from SFS samples by using an acid-base liquid-liquid extraction method with dichloromethane and distilled water. The nicotine content was quantified by HPLC/PDA (261.9 nm) with a $C_{18}$ column under a gradient of 10% acetonitrile with 20 mM ammonium formate (ammonia solution adjusted to pH 8.7) to 100% acetonitrile. The calibration curve, analyzed from concentration standards between 0.1 to 2 mg/L, presented linearity with a correlation coefficient ($r^2$)>0.9999. The limit of quantitation (LOQ) of nicotine in SFS was 0.4 mg/kg, and the average recoveries ranged from 76.4% to 96.3%. The repeatability of measurements, expressed as the coefficient of variation (CV%), ranged from 1.74 to 5.12%. This newly developed method for nicotine quantification in SFS can be considered an analytical method with an acceptable level of sensitivity and repeatability.

Effect of Sample Preparation on Predicting Chemical Composition and Fermentation Parameters in Italian ryegrass Silages by Near Infrared Spectroscopy (시료 전처리 방법이 근적외선분광법을 이용한 이탈리안 라이그라스 사일리지의 화학적 조성분 및 발효품질 평가에 미치는 영향)

  • Park, Hyung Soo;Lee, Sang Hoon;Choi, Ki Choon;Lim, Young Chul;Kim, Jong Gun;Seo, Sung;Jo, Kyu Chea
    • Journal of Animal Environmental Science
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    • v.18 no.3
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    • pp.257-266
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    • 2012
  • Near infrared reflectance spectroscopy (NIRS) has become increasingly used as a rapid, accurate method of evaluating some chemical constituents in cereal and dired animal forages. Analysis of forage quality by NIRS usually involves dry grinding samples. Costs might be reduced if samples could be analyzed without drying or grinding. The objective of this study was to investigate effect of sample preparations on prediction ability of chemical composition and fermentation parameter for Italian ryegrass silages by NIRS. A population of 147 Italian ryegrass silages representing a wide range in chemical parameters were used in this investigation. Samples were scanned at 1nm intervals over the wavelength range 680-2500 nm and the optical data recorded as log 1/Reflectance (log 1/R) and scanned in oven-dried grinding and fresh ungrinding condition. The spectral data were regressed against a range of chemical parameters using partial least squares (PLS) multivariate analysis in conjunction with four spectral math treatments to reduced the effect of extraneous noise. The optimum calibrations were selected on the basis of minimizing the standard error of cross validation (SECV) and maximizing the correlation coefficient of cross validation (${R^2}_{CV}$). The results of this study show that NIRS predicted the chemical parameters with high degree of accuracy in oven-dried grinding treatment except for moisture contents. Prediction accuracy of the moisture contents was better for fresh ungrinding treatment (SECV 1.37%, $R^2$ 0.96) than for oven-dried grinding treatments (SECV 4.31%, $R^2$ 0.68). Although the statistical indexes for accuracy of the prediction were the lower in fresh ungrinding treatment, fresh treatment may be acceptable when processing is costly or when some changes in component due to the processing are expected. Results of this experiment showed the possibility of NIRS method to predict the chemical composition and fermentation parameter of Italian ryegrass silages as routine analysis method in feeding value evaluation and for farmer advice.

Compact Orthomode Transducer for Field Experiments of Radar Backscatter at L-band (L-밴드 대역 레이더 후방 산란 측정용 소형 직교 모드 변환기)

  • Hwang, Ji-Hwan;Kwon, Soon-Gu;Joo, Jeong-Myeong;Oh, Yi-Sok
    • The Journal of Korean Institute of Electromagnetic Engineering and Science
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    • v.22 no.7
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    • pp.711-719
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    • 2011
  • A study of miniaturization of an L-band orthomode transducer(OMT) for field experiments of radar backscatter is presented in this paper. The proposed OMT is not required the additional waveguide taper structures to connect with a standard adaptor by the newly designed junction structure which bases on a waveguide taper. Total length of the OMT for L-band is about 1.2 ${\lambda}_o$(310 mm) and it's a size of 60 % of the existing OMTs. And, to increase the matching and isolation performances of each polarization, two conducting posts are inserted. The bandwidth of 420 MHz and the isolation level of about 40 dB are measured in the operating frequency. The L-band scatterometer consisting of the manufactured OMT, a horn-antenna and network analyzer(Agilent 8753E) was used STCT and 2DTST to analysis the measurement accuracy of radar backscatter. The full-polarimetric RCSs of test-target, 55 cm trihedral corner reflector, measured by the calibrated scatterometer have errors of -0.2 dB and 0.25 dB for vv-/hh-polarization, respectively. The effective isolation level is about 35.8 dB in the operating frequency. Then, the horn-antenna used to measure has the length of 300 mm, the aperture size of $450{\times}450\;mm^2$, and HPBWs of $29.5^{\circ}$ and $36.5^{\circ}$ on the principle E-/H-planes.

Vitamin C Quantification of Korean Sweet Potatoes by Cultivar and Cooking Method (국내산 고구마의 품종 및 조리방법별 비타민 C 함량)

  • Hwang, In Guk;Byun, Jae Yoon;Kim, Kyung Mi;Chung, Mi Nam;Yoo, Seon Mi
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.43 no.6
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    • pp.955-961
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    • 2014
  • This study was carried out to investigate the amounts of vitamin C in 22 sweet potato cultivars cultivated in Korea as well as evaluate the effects of cooking methods on vitamin C contents. Methods for determining vitamin C was validated by determining linearity, specificity, limit of detection (LOD), limit of quantification (LOQ), precision, and accuracy using HPLC. Results showed high linearity in the calibration curve with a coefficient of correlation ($R^2$) of 0.9999. The LOD and LOQ values for ascorbic acid (AA) were 0.03 and $0.10{\mu}g/mL$, respectively. The relative standard deviations (RSDs) for intra- and inter-day precision of AA were less than 5%. The recovery rates of AA and dehydroascorbic acid (DHA) were in the range from 98.21~98.64 and 98.28~100.68%, respectively. Depending on cultivar, contents of AA, DHA, and total ascorbic acid (TA) in sweet potatoes varied in the range from 37.76 (Sinyulmi)~89.25 (Juhwangmin), 23.37 (Sinjami)~63.94 (Sinyulmi), and 68.52 (Sinjami)~115.95 (Juhwangmin) mg/100 g, respectively, and their average levels were $56.98{\pm}12.53$, $36.46{\pm}9.03$, and $93.44{\pm}12.00mg/100g$, respectively. The average TA levels were also dependent on flesh color, whish was significantly higher in general sweet potato and orange sweet potato than in purple sweet potato. Steaming, baking, and frying processes significantly reduced AA (10.61~58.41%), DHA (2.57~52.81%), and TA (14.54~49.92%) contents in sweet potatoes. The highest reduction of AA, DHA, and TA contents was observed after baking, followed by steaming and frying. We expect that the basic information provided by this study will be useful to plant breeders and food scientists.

Modification and Validation of Analytical Method for Oxypaeoniflorin and Paeoniflorin in Moutan Cortex Radicis Extract (목단피 추출물의 Oxypaeoniflorin 및 Paeoniflorin의 분석법 개선 및 검증)

  • Choi, Seung-Hyun;Yoo, Chang-Kil;Hwang, Ji-Hyun;Lee, Gi-Bbeum;Lee, Young-Jin;Lee, Boo-Yong;Lee, Ok-Hwan
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.46 no.9
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    • pp.1091-1096
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    • 2017
  • The aim of this study was the validation of a modified analytical method for determination of oxypaeoniflorin and paeoniflorin in Moutan Cortex Radicis extract. For validation of the analytical method, we modified established analytical methods and validated improvement. For validation, the specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification of oxypaeoniflorin and paeoniflorin were measured by high performance liquid chromatography. The results show that the correlation coefficients of the calibration curve for oxypaeoniflorin and paeoniflorin were 1.0000 and 0.9998, respectively. The LOD for oxypaeoniflorin and paeoniflorin were $0.23{\mu}g/mL$ and $0.25{\mu}g/mL$, respectively. The inter-day and intra-day precision values of oxypaeoniflorin and paeoniflorin were 0.70~3.19% and 1.74~2.43%, and 0.32~0.92% and 0.62~2.28%, respectively. The inter-day and intra-day accuracies of oxypaeoniflorin and paeoniflorin were 98.33~102.11% and 97.72~118.12%, and 98.44~101.56% and 97.10~112.00%, respectively. Therefore, the analytical method was validated for the detection of oxypaeoniflorin and paeoniflorin in Moutan Cortex Radicis.

Quality Assurance Program of Electron Beams Using Thermoluminescence Dosimetry (열형광선량계를 이용한 전자선 품질보증 프로그램에 관한 연구)

  • Rah Jeong-Eun;Kim Gwe-Ya;Jeong Hee-Kyo;Shin Dong-Oh;Suh Tae-Suk
    • Progress in Medical Physics
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    • v.16 no.2
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    • pp.62-69
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    • 2005
  • The purpose of this study has been performed to investigate the possibility of external audit program using thermoluminescence dosimetry for electron beam in korea. The TLD system consists of LiF powder, type TLD-700 read with a PCL 3 reader. In order to determine a calibration coefficient of the TLD system, the reference dosimeters are irradiated to 2 Gy in a $^{60}CO$ beam at the KFDA The irradiation is performed under reference conditions is water phantom using the IAEA standard holder for TLD of electron beam. The energy correction factor is determined for LiF powder irradiated of dose to water 2 Gy in electron beams of 6, 9, 12, 16 and 20 MeV (Varian CL 2100C). The dose is determined according to the IAEA TRS-398 and by measurement with a PTW Roos type plane-parallel chamber. The TLD for each electron energy are positioned in water at reference depth. In this study, to verify of the accuracy of dose determination by the TLD system are performed through a 'blind' TLD irradiation. The results of blind test are $2.98\%,\;3.39\%\;and\;0.01\%(1\sigma)$ at 9, 16, 20 MeV, respectively. The value generally agrees within the acceptance level of $5\%$ for electron beam. The results of this study prove the possibility of the TLD quality assurance program for electron beams. It has contributed to the improvement of clinical electron dosimetry in radiotherapy centers.

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Studies on Solvent Extraction and Analytical Application of Metal-dithizone Complexes(I). Separation and Determination of Trace Heavy Metals in Urine (Dithizone 금속착물의 용매추출 및 분석적 응용(제1보). 뇨중 흔적량 중금속 원소의 분리 정량)

  • Jeon, Moon-Kyo;Choi, Jong-Moon;Kim, Young-Sang
    • Analytical Science and Technology
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    • v.9 no.4
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    • pp.336-344
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    • 1996
  • The extraction of trace cobalt, copper, nickel, cadmium, lead and zinc in urine samples of organic and alkali metal matrix into chloroform by the complex with a dithizone was studied for graphite furnace AAS determination. Various experimental conditions such as the pretreatment of urine, the pH of sample solution, and dithizone concentration in a solvent were optimized for the effective extraction, and some essential conditions were also studied for the back-extraction and digestion as well. All organic materials in 100 mL urine were destructed by the digestion with conc. $HNO_3$ 30 mL and 30% $H_2O_2$ 50 mL. Here, $H_2O_2$ was added dropwise with each 5.0 mL, serially. Analytes were extracted into 15.0 mL chloroform of 0.1% dithizone from the digested urine at pH 8.0 by shaking for 90 minutes. The pH was adjusted with a commercial buffer solution. Among analytes, cadmium, lead and zinc were back-extracted to 10.00 mL of 0.2 M $HNO_3$ from the solvent for the determination, and after the organic solvent was evaporated, others were dissolved with $HNO_3-H_2O_2$ and diluted to 10.00 mL with a deionized water. Synthetic digested urines were used to obtain optimum conditions and to plot calibration-eurves. Average recoveries of 77 to 109% for each element were obtained in sample solutions in which given amounts of analytes were added, and detection limits were Cd 0.09, Pb 0.59, Zn 0.18, Co 0.24, Cu 1.3 and Ni 1.7 ng/mL, respectively. It was concluded that this method could be applied for the determination of heavy elements in urine samples without any interferences of organic materials and major alkaline elements.

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Determination of aromatic amino acids by chemiluminometric assay with Luminol-H2O2-Cu(II) system (Luminol-H2O2-Cu(II) 시스템을 이용한 방향족 아미노산의 화학발광법적 정량)

  • Kim, Kyung-Min;Kim, Young-Ho;Lee, Sang-Hak
    • Analytical Science and Technology
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    • v.25 no.3
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    • pp.171-177
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    • 2012
  • A determination method of aromatic amino acids such as trytophan (Trp), tyrosine (Tyr), and phenylalanine (Phe) using luminol-$H_2O_2$-Cu(II) system has been presented. In the presence of an aromatic amino acid, the enhanced chemiluminescence (CL) intensity of luminol-$H_2O_2$-Cu(II) system was obtained by forming a complex between Cu(II) and the amino acid. Based on the above phenomenon, a sensitive and fast determination of three aromatic amino acids was performed using the CL method in batch-type detection system. To optimize determination conditions, the kinetic influence of an aromatic amino acid on the luminol-$H_2O_2$-Cu(II) system and the effects of $H_2O_2$ and Cu(II) concentration, pH, and buffers were investigated. Under the optimized conditions, the calibration curve was linear over the range from $1.0{\times}10^{-6}$ to $2.0{\times}10^{-5}\;M$ for Trp, $1.0{\times}10^{-6}$ to $2.0{\times}10^{-5}\;M$ for Try, and $2.0{\times}10^{-6}$ to $2.0{\times}10^{-5}\;M$ for Phe, respectively. In this range, reproducibility (RSD, n = 4) of Trp, Try, and Phe were 3.21%, 2.64%, and 2.48%, respectively. The limit of detection ($3{\sigma}/s$) was calculated to be $6.8{\times}10^{-7}\;M$ for Trp, $5.7{\times}10^{-7}\;M$ for Try, and $9.6{\times}10^{-7}\;M$ for Phe.