• 약학회지
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• 제31권5호
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• pp.315-321
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• 1987

A high performance liquid chromatographic method was developed for the determination of glycyrrhetinic acid contained in licorice powder. Glycyrrhetinic acid which is hydrolysate of glycyrrhizin extracted from licorice powder, was determined with good result by HPLC using 2-bromoacetyltriphenylene labeling reagent. The glycyrrhetinic acids were labeled with 2-bromoacetyltriphenylene in acetonitrile using 18-crown-6-ether and KOH as a catalyst. Derivatized glycyrrhetinic acids were separated from the extracted licorice powder on a reversed-phase column (chemopak $C_{18}$) using 100% acetonitrile as a mobile phase and monitored by an UV-detector at 268nm. Linearity of calibration curve was obtained between 5 ng and 20 ng, and the lower limit of detection was 2 ng. The recovery of glycyrrhetinic acid to licorice powder was about 99.3%. This method was sensitive, reliable and useful for, determination of glycyrrhetinic acid.

• Structural Engineering and Mechanics
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• 제43권1호
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• pp.127-145
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• 2012

One of the most important and challenging steps in seismic vulnerability and performance assessment of highway bridges is the determination of the bridge component damage parameters and their corresponding limit states. These parameters are very essential for defining bridge damage state as well as determining the performance of highway bridges under a seismic event. Therefore, realistic damage limit states are required in the development of reliable fragility curves, which are employed in the seismic risk assessment packages for mitigation purposes. In this article, qualitative damage assessment criteria for ordinary highway bridges are taken into account considering the critical bridge components in terms of proper engineering demand parameters (EDPs). Seismic damage of bridges is strongly related to the deformation of bridge components as well as member internal forces imposed due to seismic actions. A simple approach is proposed for determining the acceptance criteria and damage limit states for use in seismic performance and vulnerability assessment of ordinary highway bridges in Turkey constructed after the 1990s. Physical damage of bridge components is represented by three damage limit states: serviceability, damage control, and collapse prevention. Inelastic deformation and shear force demand of the bent components (column and cap beam), and superstructure displacement are the most common causes for the seismic damage of the highway bridges. Each damage limit state is quantified with respect to the EDPs: i.e. curvature and shear force demand of RC bent components and superstructure relative displacement.

• Journal of Radiation Protection and Research
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• 제35권3호
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• pp.117-123
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• 2010

Pu 동위원소는 기원에 따라 각기 다른 $^{240}Pu/^{239}Pu$ 동위원소비를 나타내는 특성이 있다. 질량분석법은 극미량 장반감기핵종 분석에 매우 유용한 방법으로서 검출기 특성상 낮은 검출한계를 갖고 있으며, 소량의 시료를 이용하여 짧은 시간에 측정을 할 수 있다는 장점을 갖고 있으므로 Pu을 비롯한 장반감기 핵종 분석에 유용하다. 다중검출기유도결합플라즈마질량분석기(Multicollector ICP-MS)는 다중검출시스템을 이용하여 분석하고자 하는 여러 핵종의 동시분석이 가능하며, 특별히 본 연구에서는 극미량 핵종의 검출이 가능한 multiple ion counter (MIC)를 사용하여 Pu 동위원소 분석에 적용하였다. 본 연구방법의 검출한계(detection limit)는 최적화된 조건에서 $^{239}Pu$와 $^{240}Pu$ 각각 $0.10\;fg\;ml^{-1}$ ($0.24\;{\mu}Bq\;ml^{-1}$), $0.12\;fg\;ml^{-1}$ ($0.97\;{\mu}Bq\;ml^{-1}$)이었으며, 240Pu 기준으로 약 200 cps 정도의 매우 낮은 농도수준에서 1%이하의 $^{240}Pu/^{239}Pu$ 동위원소비 계측편차를 나타내었다. 본 연구방법은 표준용액 및 다양한 매트릭스의 표준물질 분석에 적용함으로써 검증 확인하였다.

• Natural Product Sciences
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• 제19권1호
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• pp.20-27
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• 2013

A simple high performance liquid chromatography - diode array detector (HPLC-DAD) method has been developed and validated for simultaneous determination of the six components (cinnamic acid, cinnamaldehyde, eugenol, atractylenolide I, atractylenolide III, and ergosterol) in Oryeongsan. In addition, identification of six marker compounds was conducted by a LC-MS/MS analysis. The six compounds in Oryeongsan were separated on Shishedo $C_{18}$ column (5 ${\mu}m$, $4.6{\times}250$ mm) at a column temperature of $30^{\circ}C$. The mobile phase was a mixture of 0.1% trifluoroacetic acid (TFA) water and acetonitrile employing gradient elution at a flow rate of 1.0 mL/min. The detection wavelength was set at 205, 250, 280, and 330 nm. The developed method had good linearity ($R^2$ > 0.9997) and the limit of detection (LOD) and limit of quantification (LOQ) were observed within the ranges 0.01~0.15 and 0.05~0.45 ${\mu}g/mL$, respectively. The relative standard deviation (RSD) values of intra- and inter-day testing were indicated that less than 3% and 90.31~103.31% of accuracy. The results of recovery test were 90.56~106.72% and RSD range was measured from 0.84 to 2.95%. In conclusion, this HPLC-DAD method has been successfully applied to the simultaneous determination of six compounds in Oryeongsan samples.

• 한국환경농학회지
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• 제32권2호
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• pp.128-135
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• 2013

BACKGROUND: This study was performed to develop a single residue analytical method for new herbicide metazosulfuron in crops. METHODS AND RESULTS: Brown rice, apple, mandarin, Kimchi cabbage and soybean were selected as representative crops, and clean-up system, partition solvent and extraction solvent were optimized. Instrumental limit of quantitation (ILOQ), linearity of calibration curve and method limit of quantitation (MLOQ) were determined based on the chromatography and whole procedures. For recovery tests, brown rice, apple, mandarin, Kimchi cabbage and soybean samples were macerated and fortified with metazosulfuron standard solution at three levels (MLOQ, 10 MLOQ and 100 MLOQ). And then those were extracted with acetonitrile, concentrated, and partitioned with ethyl acetate. Then the extracts were concentrated again and cleaned-up through $NH_2$ (aminopropyl) SPE cartridge with acetone : dichloromethane (1% acetic acid) (20 : 80, v/v) before concentration and analysis with HPLC. CONCLUSION(S): ILOQ of metazosulfuron was 2 ng (S/N${\geq}$10) and good linearity was achieved between 0.05 and 12.5 mg/Kg of metazosulfuron standard solutions, with coefficients of determination of 0.9999. MLOQ was 0.02 mg/Kg. Good recoveries from 74.1 to 116.9% with coefficients of variation (C.V.) of less than 10% were obtained, regardless of sample type, which satisfies the criteria of Korea Food and Drug Administration (KFDA). Those results were reconfirmed with LC-MS (SIM). The method established in this study is simple, economic and efficient to be applied to most of crops as an official and general method for residue analysis of metazosulfuron.

• 상하수도학회지
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• 제29권4호
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• pp.493-502
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• 2015

In accordance with the Watershed Sewer System Maintenance Plan enforced on February 2, 2013, the different compliance concentration of effluent limit be applied to effluent discharged from public sewage treatment works(PSTWs) in each watershed on the basis of water quality thereof. With the introduction of watershed sewer system, it is necessary to set the compliance concentration of effluent limit for PSTWs situated in the watershed, by region and PSTW size, to achieve water quality criteria for regional watersheds or target water quality under TMDL program. Watershed Environmental Agencies establish the Watershed Sewer System Maintenance Plan and set the compliance concentrations of effluent limit for PSTWs under the plan. The agencies plan to apply tougher effluent BOD concentration limits in Class I to IV areas. Effluent BOD concentration limits will be toughened from 5~10 mg/L to 3 mg/L in class II~III areas, from 10mg/L to 5mg/L in class IV areas. Uniform application of effluent BOD concentration limits to PSTWs in the watershed sewer system need to be complemented considering type of sewage treatment technology employed and watershed characteristics. Therefore, this study presents method to determine the compliance concentration of effluent limit from PSTWs in the watershed.

• 대한화학회지
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• 제44권3호
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• pp.207-211
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• 2000

Tween80 미셀용액에서 착화제로서 APDC틀 이용하여 Ni(II)를 정량하는 방법에 대해 연구하였다. Ni(PDC)$_2$ 착물의 홉수 스펙트럼 chloroform에서 보다는 Tween80에서 더 좋은 모양과 더 좋은 감도를 보여 주었다. Ni(PDC)$_2$ 착물은 pH 7.0에서 그리고 100분 정도까지 매우 안정하였으며, APDC를 Ni(II)의 몰수의 10배 이상 넣어 주면 정량적으로 착물이 형성되었다. Tween80의 농도는 0,1%가 적절하였고,0.1% Tween80 용액에서 Ni(PDC)$_2$ 착물의 검정곡선은 좋은 직선성(R2=0.9955)을 보여주었다. 이 분석법의 검출한계와 정량한계는 각각 0.09 ${\mu}g$/mL와 0.28${\mu}g$/mL이었으며, 강물시료에 적용한 회수율은 100% 보다 조금 크게 나타났다. 비록 여러 금속이온들이 방해를 하지만, 실제시료에 들어있는 Ni(II)을 정량하는데 이용할 수 있을 것이다.

• KSBB Journal
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• 제29권4호
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• pp.232-238
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• 2014

The simultaneous determination of creatine monohydrate (CrM), dicyandiamide and dihydrotriazine in dietary supplements using reversed-phase high performance liquid chromatography (HPLC) was developed. Chromatography was performed on a Nuclosil 100-5 SA ($4.6{\times}250mm$) column with a mobile phase of 2.3% ammonium phosphate (pH 5.5), and UV detection at 224 nm, 212 nm, and 237 nm, respectively. The performance characteristics of HPLC were determined in terms of selectivity, linearity, precision, recovery, limit of detection (LOD), and limit of quantification (LOQ). The calibration curves were linear within the concentration range of $40.0{\sim}500.0{\mu}g/mL$ for creatine, $0.1{\sim}12.8{\mu}g/mL$ for dicyandiamide, and $0.05{\sim}6.4{\mu}g/mL$ for dihydrotriazine. The detection limits of the method were 1.09, 0.01, and $0.08{\mu}g/mL$ for creatine, dicyandiamide, and dihydrotriazine, respectively. The recoveries of creatine, dicyandiamide, and dihydrotriazine were 97.2~100.9, 92.3~106.5, and 97.2~105.5%, respectively. It is expected that the chromatographic analytical method developed in this study will be usefully applicable to simultaneous determination of creatine, dicyandiamide, and dihydrotriazine contained in dietary supplements.

• 분석과학
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• 제21권2호
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• pp.84-92
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• 2008

속빈 섬유-액상 미량추출법(hollow fiber-liquid phase microextraction, HF-LPME)과 기체 크로마토그래프/질소-인 검출기(GC-NPD)를 사용하여 사람의 뇨와 여러 가지 음료 중에서 극미량의 카페인을 분석하는 방법을 확립하였다. 수용액 시료로부터 카페인의 양을 측정하기 위해서 속빈 섬유의 길이, 추출용매의 종류, 교반효과, pH 및 염석효과 등 여러 가지 실험적인 파라미터를 변화시켜서 최적의 조건을 확립하고자 하였다. 검정곡선의 회귀계수($r^2$)는 0.9994이상이었으며, 평균 상대 회수율은 102%(n=3)이었으며, 기기검출한계는 2.5 ng/mL, 정량한계는 10 ng/mL이었다. 확립된 HF-LPME 방법은 생물학적 시료, 음식물, 환경시료 중에서 카페인의 농도를 측정하기에 편리하고 정확한 방법이 될 것이다.

• 약학회지
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• 제54권6호
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• pp.429-440
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• 2010

HS-SPME-GC/MS was studied and optimized for the determination of 17 orgarnophosphorous pesiticides (OPPs: chlorpyrifos, chlorpyrifos-methyl, demeton-s-methyl, diazinon, dimethoate, EPN, fenitrothion, fenthion, malathion, methidathion, monocrotophos, parathion, phenthoate, phosphamidon, sulfotep, terbufos, triazophos) in blood. Optimum SPME parameters were selected: choice of SPME fiber (85 ${\mu}m$ polyacrylate), pH effect (0.5 N HCl), salt effect ($Na_2SO_4$, 0.2 g; 20%), headspace incubation temperature ($80^{\circ}C$), headspace incubation time (1 min), headspace adsorption time (30 min) and GC desorption time (2 min). These parameters were optimized using HS-SPME autosampler coupled with gas chromatography-mass spectrometry (GC-MS). Method validation was carried out in terms of linearity, limit of detection (LOD), limit of quantitation (LOQ) and recovery in blood. The assay was linear over 0.5~5.0 mg/l ($r^2$=0.955~1.000). Limit of detection (LOD) and limit of quantitation (LOQ) in blood were determined 0.03~0.3 mg/l (S/N=3) and 0.1~1.1 mg/l (S/N=10), respectively. Relative recovery with 0.5, 1 and 5 mg/l (in blood) were 90.8%, 98.5% and 94.1%, respectively. This method will be applied to the determination of the orgarnophosphorous pesticides in postmortem blood. The proposed protocol can be an attractive alternative to be used in routine toxicological analysis.