Aralia elata Seemann (AE) has long been used as a folk medicine for the treatment of various diseases including diabetes mellitus, anti-arthritic, and anti-gastric ulcer agent in Korea, Japan, and China. This study was performed to establish a simple and reliable HPLC/UV analytical method for determination of most active anti-hypertensive compound, a 3-O-α-L-rhamnopyranosyl(1→2)-α-L-arabinopyranosyl hederagenin 28-O-β-D-xylopyranosyl(1→6)-β-D-glucopyranosylester (HE) for the standardization of the shoot extract of AE as a health functional food ingredient. The quantitative analytical method of HE was optimized by HPLC analysis using reverse-phase C18 column at 40°C with H2O and acetonitrile (70:30, v/v) as an isocratic mobile phase at a flow rate of 1.0 mL/min and detection wavelength of UV 205 nm. This HPLC/UV analytical method showed good specificity and high linearity in the tested range of 0.03125-2.0mg/ml with excellent coefficient of determination (R2) of 0.9999. The limit of detection and limit of quantification were 12.0 μg/mL and 36.5 μg/mL, respectively. Relative standard deviation (RSD) values of data from intra- and inter-day precision were less than 0.2% and 0.1%, respectively. These results indicate that the established HPLC/UV analytical method is very simple, specific, precise, accurate, and reproducible and thus can be useful for the quantitative analysis of HE as a functional anti-hypertensive compound in AE extract.

Background : Acanthopanax sessiliflorus (Rupr. et Maxim) Seem, belonging to the Araliaceae family, is widely distributed in Korea, China, and Japan. The plants belonging to Acanthopanax species are traditionally used in Korea as anti-rheumatoid arthritis, anti-inflammatory and anti-diabetic drugs and are recognized to have ginseng-like activities. A simple and sensitive high-performance liquid chromatographic (HPLC) method was developed and validated for independent analysis of major compounds and chlorogenic acid in A. sessiliflorus fruits. Chlorogenic acid was reported that prevent cancer and cardiovascular disease in vivo. Also, it has antioxidant effect in vitro test. In the previous experiment, chlorogenic acid were found in A. sessiliflorus fruits. This study was performed to identification of the major compounds and investigate the method validation for the determination of chlorogenic acid in A. sessiliflorus fruits. Methods and Results : Three major compounds were recorded on a Varian Unity Inova AS-400 FT-NMR spectrometer and analyzed by the new HPLC analysis method. HPLC analysis was carried out using an Waters e2695 and PDA detector. The new analyasis method was validated by the measurement of intra-day, inter-day precision, accuracy, limit of detection (LOD, S/N=3), and limit of quantification (LOQ, S/N=10) of chlorogenic acid. The results showed that the correlation coefficient (R2) for the calibration curves of chlorogenic acid was 0.997 in terms of linearity. The limit of detection (LOD) and limit of quantification (LOQ) were 0.565 ㎍/ml and 2.88 ㎍/ml, respectively. There was no interfering peak observed each other and HPLC system was suitable for analysis showing goodness of peak and high precision. Conclusion : This method is suitable to detect and quantify major compounds in A. sessiliflorus fruits. Furthermore, the result will be applied to establish chlorogenic acid as an standard compound for A. sessiliflorus fruits.

Background : Cynanchum wilfordii and Cynanchum auriculatum belong to the Asclepiadaceae family and appear morphologically similar. In order to discriminate them, it is needed to find the presence of sap and the leaf shapes: C. auriculatum has a blade ovate leaf comparing to C. wilfordii. However, in the herbal medicine market, they have been handled as cut and dried roots. Due to their similar morphology, it is limited to distinguish the roots of C. wilfordii and C. auriculatum. Recently in Korea, it has been a critical issue to misuse these two roots in the herbal market and food industry. Thus, it is required to establish a robust tool for the discrimination and quality control of them. Methods and Results : To separation and characterization of flavor compounds, C. wilfordii and C. auriculatum samples were analyzed by head space solid phase micro extraction (HSS) fiber coupled with gas chromatography-mass spectrometry using Rtx-5MS (30 m x 0.25 mm x 0.25 μm) column. As a result, We have identified compounds of a few hundred in aliphatic aldehydes and aliphatic alcohols, alkenes and acids, aromatic compounds, aromatic compounds containing nitrogen & sulfur, etc,. In particular, The aliphatic and aromatic compounds had been clearly separated on the second dimensional direction by using two-dimensional GC. Conclusion : The volatile flavor compounds of C. wilfordii and C. auriculatum could easily analyzed without pre-treatment with improved resolution and sensitivity using HSS-GCxGC-TOFMS. We have identified compounds of a few hundred in C. wilfordii and C. auriculatum sample. And It was more accurately qualitative confirmed with separation of GCxGC and TSD. We have confirmed the PCA and PLS-DA Plot that was classified depending on C. wilfordii and C. auriculatum through multivariate statistical analysis of the identified flavor compounds.

Between the RC and SC structures, the connection method, such as baseplate type(mechanical splice) & noncontact lap splices, was suggested in KEPIC SNG. In previous research, baseplate type using #14bar were developed and their structural integrity was confirmed by the actual bending test. However, the structural integrity of noncontact lap splices using #14bar has not been yet confirmed through experiment. In this study, load-displacement curve of noncontact lap splices FEM model is compared with baseplate type analytical results. This research suggests the possibility of the noncontact lap splice for connection design in case of #14 dowel bar of RC Structure.

Background: In the present study, we established an HPLC (high performance liquid chromatography)-analysis method for the determination of marker compounds as a part of the material standardization for the development of health-functional foods from Salvia plebeia R. Br. extract. Methods and Results: The quantitative determination method of hispidulin as a marker compound was optimized by HPLC analysis using a YMC hydrosphere C18 column with a gradient elution system. This method was validated using specificity, linearity, accuracy, and precision tests. It showed a high linearity in the calibration curve with a coefficient of correlation (r2) of 0.999995. The method was fully validated, and was sensitive, with the limit of detection (LOD) at 0.09 ㎍• ㎖−1 and limit of quantification (LOQ) at 0.27 ㎍• ㎖−1. The relative standard deviation (RSD) values of the data from intra- and inter-day precision were 0.05 - 0.22% and 0.32 - 0.42%, respectively, and the intra- and inter-day accuracy of hispidulin were 99.5 - 102.3% and 98.8 - 101.5%, respectively. The average content of hispidulin in Salvia plebeia R. Br. extract was 3.945 ㎎• g−1 (0.39%). Conclusions: These results suggest that the developed HPLC method is very efficient, and that it could contribute to the quality control of Salvia plebeia R. Br. extracts as a functional ingredient in health functional foods.

Background: Cyanazine is used as a pre-emergent herbicide once during the growing season to control weeds of many upland crops worldwide. This study aimed to establish a method to determined cyanazine residue levels in major medicinal crops by using high performance liquid chromatography-UV detection/mass spectometry (HPLC-UVD/MS). Methods and Results: Cyanazine residue was extracted with acetone from the raw products of four representative medicinal plants - Scutellaria baicalensis, Paeonia lactiflora, Platycodon grandiflorum and Angelica gigas. The extract was diluted with a large volume of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. It was then purifined using optimized Florisil column chromatography. HPLC analysis conducted using an octadecylsilyl column allowed the successful separation of cyanazine from co-extractives of the samples, and the amount was sensitively quantified by ultraviolet absorption at 225 ㎚ with no interference. The accuracy and precision of the proposed method were validated by conducting recovery experiments on each medicinal crop sample fortified with cyanazine at two concentration levels per crop in triplicate. Conclusions: The mean recoveries ranged from 91.2% to 105.3% for the four representative medicinal crops. The coefficients of variation were less than 10%, irrespective of the sample types and fortification levels. The limit of quantification of cyanazine was 0.02 ㎎/㎏ as verified by the recovery experiment. A confirmatory method was performed by liquid chromatography/MS using selected-ion monitoring technique to clearly identify the suspected residue.

The analytical method for 16 organophosphorus pesticides was developed in this study. The 16 organophosphorus pesticides were analyzed by liquid chromatography-tandem mass spectrometry (LC/MS/MS) using on-line solid phase extraction (on-line SPE) with PLRP- S cartridge. Analysis of all analytes in the MS/MS was processed in the electrospray ioni-zation (ESI) positive mode. They are Azinphos ethyl, Chlorfenvinphos, Ethion, Famphur, Phosmet, Phosphamidon, Terbufos, Aspon, Chlorpyrifos-methyl, Crotoxyphos, Dichlofenthi-on, Dicrotophos, Fonofos, Thionazin, Dimethoate and Iprobenfos. Limits of detection (LODs) and Limits of quantification(LOQs) were obtained as 0.8~2.0 ng/L and 2.6~6.4 ng/L, respectively. All compounds were not detected at the 8 sampling points of the raw water and clean water.

This study aims to apply multistage homotopy perturbation method (MHPM) to SDOF space truss to obtain a semi-analytical solution. For the purpose, a nonlinear governing equation is derived in consideration of geometrical nonlinearity, and homotopy equation is formulated. The result of carrying out dynamic analysis on a simple model is compared to a numerical method of 4th order Runge-Kutta method (RK4), and the dynamic response by MHPM concurs with the numerical result.

This paper presents an analytical approach to evaluate a possibility of progressive collapse of reinforced concrete frame structure. In order to simulate adequate behavior of the structure, we considered the bond failure of lap spliced bars due to concrete crack in a plastic hinge region. Analysis result gave that there was additional deflection due to the bond failure of bar in beams at the node where the increasing displacement load was applied. The stress was concentrated to the beam where a column was removed, and as it goes up to higher stories, the moment change of an upper story appeared less.

This study was conducted to improve the analytical method of siloxanes in biogas. Methanol and hexane were tested as absorption solvents of the impinger absorption method, and also the hexane extraction for pretreatment of sample was evaluated. Manufactured gas contained siloxanes of 50 ppm was completely absorbed by the methanol impinger absorption. The absorption efficiency of biogas containing only 2 ppm, however, was maximum 84%. As the condensate on the first impinger increased, the absorption rate of methanol was decreased. The hexane extraction method of the sample was considered to proper the method of moisture removal. The hexane extraction result showed the high recovery factor and the low relative standard deviation. It is suggested that the suitable choice of solvent and pretreatment is required, as the analysis result of siloxane sample may be differentiated depending on the type of biogas or the sampling point.

It is important to understand the trajectory of structure in launching process because of the short time of launching process may result in unexpected accidents or damage to structures. The high risk of structural failure is not avoidable without the fully comprehension of changing forces in launching procedure. The commercial software can evaluate the motion of launching event in calm water condition but there is the limitation of research application because of the programmed commercial software. The launching process of the spar hull is suggested with stage concept that is divided into 10 stages in time domain. A force equilibrium diagram is derived for each stage where the changes of force vector and motion characteristics take place. In particular, the effects of changes in buoyancy and drag force due to the progressive submergence of the spar hull are taken into account by means of a touch length concept. The results contained in this paper provide the valuable information of the trajectory motion evaluation with suggested methods in spar launching process with sliding barge. Furthermore, the presented stage concept and touch length concept will provide basic knowledge for understanding launching process and help to develop further research area for launching analysis.

본 연구에서는 해석의 결과 내부 지점부 보강과 외부프리스트레싱의 도입이 일반 플레이트거더교의 단면보다 단면감소의 효과가 있음을 확인하였으며 특히 외부프리스트레싱의 도입으로 얻은 솟음은 교량의 처짐을 감소시켜 사용성 측면에서 긍정적인 효과를 나타냄을 확인하였다. 해석결과를 바탕으로 하여 거더 개수 별 적용가능 단면을 도시 하였으며, 거더 개수가 4개일 경우에 한하여 회귀분석을 시행해 회귀식을 제시함으로써 추후에 이와 같은 단면을 사용할 때 응력예측을 가능할 수 있게 하였다.

The simultaneous determination of residual pesticides was developed using a gas chromatography. In this study, a simple and reliable methodology was improved to detect 175 kinds of residual pesticides by a liquid-liquid extraction procedure, followed by chromatographic analysis by gas chromatography. The 175 kinds of residual pesticides was classified into 4 groups according to the chemical structure, column type, resolution and sensitivity. The soybean sample selected for recovery experiment was not detected any pesticides. The recovery rates were ranged from 70.6% to 119.7% in most pesticides. The relative standard deviation (RSD 0.3~5.6%) was lower than 5.6% in all cases. The limits of detection (LOD) was lower than the maximum residue levels established by Korean legislations. The method has been successfully applied to the analysis of approximately 130 real samples.

프탈레이트는 화장품 원료로서 사용되지 않지만 네일락카, 헤어스프레이 제품류 등에는 혼입 또는 오염에 의해 제품 중에서 검출되어 시민단체 등에 의해 지속적인 안전성 문제가 제기되고 있기에 이들 제품에 대한 정확한 함량분석은 매우 중요하다. 그러나, 대부분의 프탈레이트 시험은 수질 또는 환경시료 등에서 다량의 유기용매로 추출/농축하여 가스크로마토그래피-질량분광분석기(GC-MS)를 사용하여 미량의 함량을 분석하는 방법으로 화장품 분석에 적용하기가 쉽지 않으며 화장품 분석에 적용되는 공인시험법도 아직까지 없는 실정이다. 또한 질량분석기의 가격, 시료전처리 및 기기유지관리에 소요되는 비용과 시간이 적지 않아 일반적인 품질관리에 적용하기엔 부담이 적지 않다. 특히 프탈레이트의 ppm 수준 이하 농도 분석시에는 기기 및 기구, 시약 등의 오염에 의해 분석결과 수치가 높게 나타나는 문제점으로 인해 정확한 분석기술과 분석경험이 매우 중요하다. 이에 본 연구에서는 네일락카와 헤어스프레이 제품 분석에 적합하며 품질보증(quality-assurance ; Q.A)을 위한 시험에도 유용하도록 저비용의 범용적인 기기를 사용하면서 ppm 농도의 프탈레이트를 빠른 시간에 분석할 수 있는 방법을 설계하였다. 이 방법은 유기용매 사용량을 최소화하여 친환경적이며, 시료전처리 시간과 단계를 줄여 오염의 가능성을 최소화하며 저비용의 가스크로마토그래피-불꽃이온화검출기(GC-FID)를 사용하여 제품 내 2 ∼ 50 g/g (ppm) 농도의 프탈레이트를 검출하는 분석법으로 관련업체에서 매우 유용하게 사용될 수 있을 것이다.

종실에 비해 다량의 rutin이 함유된 것으로 알려진 메밀 식물체의 최적 rutin함량 분석조건을 확립하기 위해 추출조건, HPLC 분석조건, 분석 재현성 및 최소검출한계를 검토한 결과 rutin은 미황색을 나타내는 폴리페놀 성분으로 에탄올에 용해 하여 최대 흡수파장을 측정하였을 때 359nm에서 흡수 극대파장을 나타내었다. 메밀 식물체 함유 rutin의 최적 HPLC분석 조건을 검토한 결과 컬럼은 Tosoh ODS 120T를 이용하고, 검출기 파장을 355nm, 이동상으로 A용매를 2~% 초산함유-45~% 아세토나이트릴로, B용매는 2~% 초산함유-증류수로 하여 농도구배조건을 0분 : 50~% A용액, 0-18분 : 100~% A용액, 18-20분 : 50~% A용액, 20-22분 : 50~% A용액으로 조절하고, 분당 1mL를 용출 하였을 때 가장 우수한 분리가 유도되는 것을 확인할 수 있었다. 또한 HPLC 분석요인에 대한 재현성을 검정한 결과 머무름시간, peak면적 및 peak높이의 변이 계수가 모두 0.6~% 미만을 나타내어 극히 높은 분석 재현성을 나타내는 것으로 조사되었으며, HPLC분석 시 최소검출한계는 20ng/mL수준이었다. 메밀 식물체 함유 rutin 분석을 위한 최적 추출조건을 검토한 결과 추출용매를 에탄올로 사용하고, 80℃ 조건에서 120분 이상의 환류추출을 시행하는 것이 가장 바람직한 추출법으로 조사되었다

Quinclorac, bentazone, 2,4-D, bensulfuron-methyl, dymuron, capropamide, pencycuron 및 ethofenprox를 동시에 분석할 수 있는 전처리 방법과 0.1% 인산 및 아세토니트릴을 이동상으로하고 225 nm를 측정파장으로 사용한 RP-HPLC(reverse phase-high performance liquid chromatography)법을 개발하였다. 동 농약성분들의 검출 및 정량한계는 각각 0.12〜0.84 ppm 및 0.34〜1.20 ppm이었고, 회수율은 78〜96%이었다. 본 방법을 통하여 시료 전처리에서 분석까지 기존 13시간이 소요된 총 분석시간을 3시간 이내로 줄일 수 있었다.

A new method based on solid phase microextraction(SPME), coupled with GC/FID, has been developed for the determination of PCE and TCE in water samples. The experimental parameters affecting the SPME process (i.e, kinds of fibers, extraction time, desorption time, extraction temperature, volume ratio of sample to headspace, salt addition, and magnetic stirring) were optimized. The coefficients of determination (R2) for PCE and TCE were 0.9951 and 0.9831, respectively when analytes concentration ranges from 10 to 300㎍/L. The relative standard deviations were 3.4 and 2.1% for concentration of 10㎍/L(n=5), respectively. The detection limits of PCE and TCE were 0.5 and 1.3㎍/L, respectively.