• Title/Summary/Keyword: simple analytical method

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Isolation, Quality Evaluation, and Seasonal Changes of Bakkenolide B in Petasites japonicus by HPLC (머위로부터 Bakkenolide B의 순수분리, HPLC분석 방법 및 채취 시기별 함량 분석)

  • Kim, Tae Hoon;Kim, Do Youn;Jung, Won Jung;Nagaiya, Ravichandran;Son, Beung Gu;Park, Young Hoon;Kang, Jum Soon;Lee, Young Jae;Im, Dong-Soon;Lee, Young-Geun;Choi, Yung Hyun;Choi, Young-Whan
    • Journal of Life Science
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    • v.24 no.3
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    • pp.252-259
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    • 2014
  • The leaves of Peatasites japonicus are a traditional oriental medicine with diverse biological activities. A simple and specific analytical method for the quantitative determination of bakkenolide B constituents from methanolic extract of the leaves of P. japonicus was developed. Bakkenolide B was isolated from the leaves of P. japonicus, and its structure was elucidated based on 1D, 2D NMR, and GC-MS spectral data. A liquid chromatographic method was developed to evaluate the quality of P. japonicus through determination of major active compound, bakkenolide B. The wavelengths at 254 and 215 nm were chosen to determine bakkenolide B. The recovery of the method was in the range of 98.6 to 103.1%, and bakkenolide B showed good linearity ($r^2$=0.999) within test ranges. The developed method was applied to the determination of bakkenolide B in the plant part and seasonal changes. The results showed that the content of bakkenolide B in the leaf was higher than in the petiole and rhizome. In this study, a simple, rapid, and reliable high-performance liquid chromatography method was used to determine the percentage and composition of bakkenolide B in P. japonicus procured from different Petasites species plants in South Korea. The method can be employed in routine quantitative analysis and quality control of different products in the market.

Simultaneous Determination of Chromium (III) and Chromium(VI) by High Performance Liquid Chromatography(HPLC) (고성능 액체크로마토그래피(HPLC)를 이용한 3가, 6가 크롬의 동시정량에 관한 연구)

  • Roh, Jae Hoon;Kim, Chi Nyon;Kim, Choon Sung;Kim, Kyoo Sang
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.4 no.2
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    • pp.189-197
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    • 1994
  • Analytic methods for Cr(VI) level in industrial hygienic field were suggested by the National Institute for Occupational Safety and Health(NIOSH method 7600, 7604). There were growing needs for measurement of Cr(III) and Cr(VI) levels simultaneously. Two analytical methods were suggested to determine Cr(III) and Cr(VI) levels simultaneously. The one is method by using reversed phase high peformance liquid chromatography(HPLC) and the other is by using ion exchange HPLC. The purpose of this work was to evaluate the usefulness of these two analytic methods. For the difference of ionic charges of Cr(III)-ethylendiamine tetraacetic acid(EDTA) chelate and $CrO_4{^-2}$, we could detect them simultaneously by ion exchange HPLC. Also, we attempted to determine the levels of Cr(III) and Cr(VI) chelated with sodium diethyldithiocarbamate(NaDDTC) by using reversed phase HPLC. The confirmation of Cr(III) and Cr(VI) were checked by fraction collector and nameless atomic absorption spectrometer. The optimal conditions for the formation of Cr(III)-EDTA chelate were two hours incubation period with pH 5. Cr(III)-EDTA and Cr(VI) in EDTA solution were successfully separated by anion exchange column using $Na_2CO_3/NaOH$ mixture as mobile phase. Peaks of Cr(III)-EDTA and Cr(VI) in EDTA were identified at 5 minutes and 7 minutes of retention time respectively by the ion exchange HPLC. The formation of Cr(III)-NaDDTC and Cr(VI)-NaDDTC chelates were twelve hours incubation period. Cr(III)-NaDDTC and Cr(VI)-NaDDTC chelates were separated by reversed phase column using methanol and water mixture as mobile phase. Peaks of Cr(VI)NaDDTC and Cr(III)-NaDDTC chelates were identified at 13 minutes and 26 minutes of retention time respectively by the reversed phase HPLC. Due to reduction of Cr(VI) to Cr(III), it seems to be not suitable for simultaneous determination of Cr(III)-NaDDTC and Cr(VI)-NaDDTC chelates by reversed phase HPLS. Simultaneos determination of Cr(III) and Cr(VI) by ion exchange HPLC was more accurate and simple method.

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Development of the analytical method for pesticide residues in crops by using gas chromatograph / solvent free solid injector (GC / SFSI) (무용매 고체 시료 주입기(SFSI)를 이용한 작물 중 잔류농약의 기체크로마토그래피 분석법 개발)

  • Kim, M.R.;Lee, Y.;Park, B.J.;Choi, J.H.;Kim, I.S.;Shim, J.H.
    • The Korean Journal of Pesticide Science
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    • v.9 no.3
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    • pp.237-242
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    • 2005
  • This experiment was carried out to develop the fast and simple method for pesticide residue analysis by using solvent free solid injector (SFSI) and to validate the efficiency of the method developed for the residue analysis of the endocrine disruptor-like pesticides such as endosulfan, metribuzin, trifluralin and vinclozolin. The samples after freeze drying were sealed in glass capillary tubes and then introduced into the heated injector of gas chromatogaphy. The required pre-heating times were 1 min for endosulfan and trifluralin, 5 min for vinclozolin, and 10 min for metribuzin. The detection limits of endosulfan in chinese cabbages, metribuzin in lettuces, trifluralin in spinachs and vinclozolin in hot peppers were 0.05, 0.1, 0.05 and 0.05 ng, respectively and their recoveries were ranged from 74%, $98{\sim}107%$, $86{\sim}95%$ and $94{\sim}95%$, respectively. The detected level of metribuzine residue in field lettuce samples by using the SFSI was 0.6 ng/mg.

Determination of Niacin in Infant Formula by Solid-phase Clean-up and HPLC with Photodiode Array Detector (고체상 정제 및 HPLC/PDA에 의한 영유아식 중 나이아신의 분석)

  • Hong, Jee-Eun;Kim, Mi-Ran;Cheon, Sang-Hee;Chai, Jung-Young;Park, Eun-Ryong;Mun, Chun-Sun;Gwak, In-Shin;Kim, Ok-Hee;Lee, Kwang-Ho
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.38 no.3
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    • pp.359-363
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    • 2009
  • This study was performed to establish a rapid and simple analytical method for niacin (nicotinic acid and nicotinamide) using HPLC. A pretreatment method for the extraction and clean-up of niacin in infant formula sample and an instrumental condition for HPLC were optimized. Niacin was extracted by 5 mM hexanesulfonate with ultrasonication for 30 min. For the clean-up of the sample, the extract was applied to a HLB cartridge, and then niacin was eluted from the cartridge using 5 mL of 80% methanol after washing with 5 mL of n-hexane. The total recoveries were $83{\sim}104%$ and relative standard deviation were in the range of $1.5{\sim}3.5%$ during the extraction and clean-up process. Niacin was determined by gradient elution with sodium hexanesulfonate/methanol buffer as a mobile phase and a photodiode array detector (260 nm). It showed a high linearity between the content of niacin and the peak area ($r^2$=1.000) in the range of $0.02{\sim}10.0$ mg/L of nicotinic acid and nicotinamide. The detection limit was 0.02 mg/L (0.2 mg/kg in the sample). The method was successfully applied for the determination of niacin in infant formula. Total niacin contents were in the range of $53.5{\sim}140.3$ mg/kg.

Simultaneous determination of 11-nor-Δ9-carboxy-tetrahydrocannabinol and 11-nor-Δ9-carboxy-tetrahydrocannabinol-glucuronide in urine samples by LC-MS/MS and its application to forensic science (LC-MS/MS를 이용한 소변 중 11-nor-Δ9-carboxy-tetrahydrocannabinol 및 11-nor-Δ9-carboxy-tetrahydrocannabinol-glucuronide의 동시 분석 및 법과학적 적용)

  • Park, Meejung;Kim, Sineun
    • Analytical Science and Technology
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    • v.34 no.6
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    • pp.259-266
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    • 2021
  • Cannabis (Marijuana) is one of the most widely used drugs in the world, and its distribution has been controlled in South Korea since 1976. Identification of 11-nor-Δ9-carboxy-tetrahydrocannabinol (THCCOOH) in urine can provide important proof of cannabis use, and it is considered scientific evidence in the forensic field. In this study, we describe a simultaneous quantitative method for identifying THCCOOH and THCCOOH-glucuronide in urine, using simple liquid-liquid extraction (LLE), and liquid chromatography-tandem mass spectrometry (LC-MS/MS). THCCOOH-D3 and THCCOOH-glucuronide-D3 were used as internal standards. Validation results of the matrix effect, as well as recovery, linearity, precision, accuracy, process efficiency, and stability were all satisfactory. No carryover, endogenous or exogenous interferences were observed. The limit of detection (LOD) of THCCOOH and THCCOOH-glucuronide were 0.3 and 0.2 ng/mL, respectively. The developed method was applied to 28 authentic human urine samples that tested positive in immunoassay screening and gas chromatography/mass spectrometry (GC/MS) tests. The ranges of concentrations of THCCOOH and THCCOOH-glucuronide in the samples were less than LOQ~266.90 ng/mL and 6.43~2133.03 ng/mL, respectively. The concentrations of THCCOOH-glucuronide were higher than those of THCCOOH in all samples. This method can be effectively and successfully applied for the confirmation of cannabinoid use in human urine samples in the forensic field.

Establishment of Pre-Harvest Residue Limit(PHRL) of the Fungicide Amisulbrom during Cultivation of Winter-Grown Cabbage (엇갈이배추 재배기간 중 살균제 Amisulbrom의 생산단계 잔류허용기준 설정)

  • Ahn, Kyung-Geun;Kim, Gyeong-Ha;Kim, Gi-Ppeum;Kim, Min-Ji;Hong, Seung-Beom;Hwang, Young-Sun;Kwon, Chan-Hyeok;Son, Young Wook;Lee, Young Deuk;Choung, Myoung-Gun
    • Korean Journal of Environmental Agriculture
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    • v.34 no.2
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    • pp.120-127
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    • 2015
  • BACKGROUND: Supervised residue trials were conducted to establish pre-harvest residue limit(PHRL), a criterion to ensure the safety of the pesticide residue in the crop harvest, of amisulbrom for winter-grown cabbage in two fields. Following to application of amisulbrom on the crop, time-course study was carried out to obtain the amisulbrom dissipation of statistical significance which enabled to calculate the predicted values of PHRL. METHOD AND RESULTS: During cultivation under greenhouse condition, samples of winter-grown cabbage were collected at 0, 1, 3, 5, 7 and 10 days after amisulbrom application, and subjected to residue analysis. Analytical method was validated by recoveries ranging 93.7~100.0% as well as limit of quantitation(LOQ) of 0.04 mg/kg. Amisulbrom residues in winter-grown cabbage gradually decreased as time elapsed. The dissipation rate of the residue would be affected by intrinsic degradation along with dilution by the cabbage growth. The decay pattern was well fitted by the simple first-order kinetics. CONCLUSION: Biological half-lives of amisulbrom in winter-grown cabbage ranged 3.7~4.1 days in two field conditions. Based on the regression of amisulbrom dissipation, PHRLs of amisulbrom in winter-grown cabbage were recommended as 8.86~9.47 and 4.21~4.35 mg/kg for 10 and 5 days before harvest, respectively.

A Fundamental Study on Evaluation of Web Crippling Strength of Corroded H-Beams (부식 H형 강재의 복부좌굴강도 추정에 관한 기초적 연구)

  • Kim, In-Tae;Shin, Chang-Hee;Cheung, Ji-Young
    • Journal of Korean Society of Steel Construction
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    • v.22 no.5
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    • pp.421-433
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    • 2010
  • The most typical deterioration of steel structures is corrosion damage. However, a method to evaluate residual load-carrying capacity of corroded steel structures is not yet established. It is difficult to check current serviceability and safety of the structures. In this study, compressive tests and finite element analyses were conducted on H-beams with corroded web. Then, the effect of corrosion damage on web crippling strength and evaluation methods of the web crippling strength are studied. Based on the tests, 4 H-beam specimens used in a subway construction site and 9 H-beam specimens with different web-thickness and damaged-height underwent compression-tests. To consider loading and supporting areas in the site, compressive loading was applied in the entire region of the upper and bottom flange in 5 H-beam specimens and applied partially on the regions of the upper and bottom flange in 8 specimens. The finite element analysis of 38 parametric model specimens simulating different corrosion damages was also carried out. From experimental and analytical results, the relationships between corrosion damages in the web and residual web crippling strength are presented. Factors web crippling strength was reduced are formulated by using residual average thickness and the standard deviation of the corroded web thickness. Also, a simple evaluation method of residual web crippling strength was proposed.

The Second-order Scattering of the Interaction of Pd Nanoparticles with Protein and Its Analytical Application

  • Guo, Xiaoyan;He, Baolin;Sun, Chuntao;Zhao, Yanxi;Huang, Tao;Liew, Kongyong;Liu, Hanfan
    • Bulletin of the Korean Chemical Society
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    • v.28 no.10
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    • pp.1746-1750
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    • 2007
  • The second-order scattering (SOS) phenomenon of the interaction of Pd nanoparticles with protein was reported and a simple, sensitive, palladium nanoparticle-based assay for trace amount of protein with SOS technique was developed. The SOS intensities were significantly enhanced due to the interaction of Pd nanoparticles with bovine serum albumin (BSA) or human serum albumin (HSA) at pH 3.5 or 4.0, respectively. The maximum SOS peak appeared at 260/520 nm (λex/λem). The optimal experiment conditions, affecting factors and the influence of some coexisting substances were checked. The SOS intensity increased proportionally with the increase of Pd concentration below 3.0 × 10?5 mol·L?1, while declined gradually above 4.0 × 10?5 mol·L?1. BSA within the range of 0.01-2.6 μg·mL?1 and HSA of 0.01-1.7 μg·mL?1 can be detected with this method and the detection limits were 2.3 and 11.2 ng·mL?1, respectively. The method was successfully applied to the quantitative detection of total protein content in human serum samples with the maximum relative standard deviation (RSD) lower than 2.6% and the recoveries over the range of 99.5-100.5%.

A Study on the Natural Frequency of Wind Turbine Tower Regarding to Modeling Method (풍력터빈타워의 모델링에 따른 고유진동수 특성에 관한 연구)

  • Lee, Yun-Woo;Jang, Min-Seo;Kang, Soung-Yong;Kim, Pyoung-Hwa;Kang, Young-Jong
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.16 no.3
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    • pp.2272-2278
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    • 2015
  • Recently the importance of renewable energy is stood out regarding to the international concern about global environmental issues. Wind power is beginning to receive attention as one of renewable energy, and world-wide researches about wind power are being carried out. In the wind power system, tower structure plays an important roles for continuous and stable generation of electricity. Researchers use various analytical models to research and develop about tower structures. In this study, the effects of natural frequencies of various wind turbine tower models have been analyzed. It is possible to simplify the detailed parts of models by using modified tower unit weight since the results of 1st natural frequency show that the difference is only 0.14%. Since the difference in natural frequency is greater than 10%, according to the boundary condition, the simple fix end support is not appropriate to represent the real structure of the tower. It is expected that the result of this study may be utilized to establish the criterion about appropriate modelling method.

Simultaneous Analysis of Pesticides in Aqueous Sample by HF-LPME (HF-LPME를 이용한 수용액 시료 내 농약의 동시 분석)

  • Nam, Jang-Woo;Lee, Kang-Jin;Myung, Seung-Woon
    • Journal of the Korean Chemical Society
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    • v.56 no.5
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    • pp.583-590
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    • 2012
  • The HF (Hollow fiber) extraction method was optimized to analysis seven species of pesticides in aqueous sample and analyzing samples by GC/MS. Hollow fiber extraction showed good efficiency when it was conducted under these conditions: organic solvent was toluene and agitation speed was 1200 rpm. The 15% concentration of NaCl was optimized when it was experimented between 5% and 25%. The equilibrium time was determined at 15 minutes. The pH 5 showed the best effect on the extraction efficiency. The linearities of calibration curves of seven species were good with correlation of regression ($r^2$) over 0.995 when they were experimented over a concentration range of $5{\mu}g/L$ to $50{\mu}g/L$. The analytical data exhibited the detection of limits (LODs) range of $0.37{\mu}g/L$ to $1.23{\mu}g/L$ and the limit of quantification (LOQs) range of $1.19{\mu}g/L$ to $3.91{\mu}g/L$. The optimized HF-LPME extraction method provides a simple and effective preparation and requires small amount of organic solvents and samples compared to conventional pre-treatment methods.