• 한국환경농학회지
• /
• 제23권4호
• /
• pp.251-257
• /
• 2004

Analytical methods were developed to determine cyclosulfamuron residues in soil, water, rice grain and straw using high-performance liquid chromatography (HPLC) with ultraviolet absorption detection. In these methods, cyclosulfamuron was extracted with aqueous $Na_2HPO_4$/acetone and acetone/methanol mixture from soil and rice samples respectively. Liquid-liquid partition coupled with ion-associated technique, Florisil column chromatography, and solid-phase extraction (SPE) were used to separate cyclosulfamuron from interfering co-extractives prior to HPLC analysis. For water sample, the residue was enriched in $C_{18}$-SPE cartridge, cleaned up in situ, and directly subjected to HPLC. Reverse-phase HPLC under ion-suppression was successfully applied to determine cyclo-sulfamuron in sample extracts with the detection at its ${\lambda}_{max}$ (254 nm). Recoveries from fortified samples averaged $87.8{\pm}7.1%$ (n=12), $97.3{\pm}7.2%$ (n=12), $90.8{\pm}6.6%$ (n=6), and $78.5{\pm}6.7%$ (n=6) for soil, water, rice grain and straw, respectively. Detection limits of the methods were 0.004 mg/kg, 0.001 mg/L, 0.01 mg/kg and 0.02 mg/kg for soil, water, rice grain and straw samples, respectively.

• 한국재료학회지
• /
• 제16권11호
• /
• pp.663-667
• /
• 2006

CTAB(cetyltrimethylammonium bromide)-capped CdSe nanoparticles were prepared by using a 4 : 1(v/v) distilled water-isopropyl alcohol mixture. The cadmium chloride and sodium selenosulfate were used as the cadmium and selenium source. By the analysis of XRD and XPS, the resultant particle was confirmed to be cubic CdSe phase. TEM image showed CdSe nanoparticles with empty core. The CTAB-capped sample showed an maximum absorption at 418nm, blue-shifting compared with bulk CdSe, which indicated stronger quantum confinement effect compared with uncapped sample. From FT-IR analysis, it was found that the presence of the new peaks in the $850{\sim}1250cm^{-1}$ range indicated the existence of chemical bonding between CTAB and surface of CdSe nanoparticles. Also TG analysis indicated that there were two weight-loss steps for the CTAB-capped CdSe nanoparticles. It was suggested that CTAB played a significant role in protecting CdSe nanoparticles.

• 한국식품과학회지
• /
• 제48권1호
• /
• pp.15-19
• /
• 2016

Drying process was applied to increase the antioxidant activity of onion powder: freeze-drying or air-drying at 50, 70, and $90^{\circ}C$ and onion extracts were obtained from each powder using water or aqueous ethanol (50%) at $25^{\circ}C$ and $60^{\circ}C$. In the color analysis, the freeze-dried powders showed higher $L^*$ and lower $a^*$ and $b^*$ values than did the air-dried ones. The browning index of powders air-dried at $90^{\circ}C$ was significantly higher than that of freeze-dried powders or those air-dried at temperatures below $90^{\circ}C$. Phenolic content in the extracts was 4.02-23.12 mg gallic acid equivalent/g sample, and was the highest in the extract from the sample air-dried at $90^{\circ}C$, regardless of the extraction condition. The highest antioxidant activity, measured by 2,2-azinobis-3-ethylbenzothiazoline-6-sulfonic acid and 1,1-diphenyl-2-picrylhydrazyl methods, was found in the powder air-dried at $90^{\circ}C$, which induced browning. These findings indicate that antioxidant activity depends more on browning during drying than on extraction conditions.

• 공업화학
• /
• 제30권5호
• /
• pp.562-568
• /
• 2019

Cylindrical shape extrudates of calcium silicate hydrate (CSH) were prepared using different percentages of polyvinyl alcohol (PVA) / sodium alginate (SA) mixtures as binders and an aqueous solution containing 6% $H_3BO_3$ and 3% $CaCl_2$ was used as a cross linking agent. As the quantity of alginate increases, the phosphate removal efficiency and capacity were decreased. Among four different extrudate samples, the sample prepared by 8% PVA + 2% SA showed the highest phosphate removal efficiency (59.59%) and capacity (29.97 mg/g) at an initial phosphate concentration of 100 ppm and 2.0 g/L adsorbent dosage. Effects of the adsorbent dosage, contact time and initial phosphate concentration on the sample were further studied. The removal efficiency and capacity obtained by a 4.0 g/L adsorbent dose at an initial phosphate concentration of 100 ppm in 3 h were 79.38% and 19.96 mg/g, respectively. The experimental data of kinetic and isotherm measurements followed the pseudo-second-order kinetic equation and Langmuir isotherm model, respectively. These results suggested that the phosphate removal was processed via a chemisorption and a monolayer coverage of phosphate anions was on the CSH surface. The maximum adsorption capacity ($q_{max}$) was calculated as 23.87 mg/g from Langmuir isotherm model.

• 약학회지
• /
• 제5권1호
• /
• pp.20-23
• /
• 1960

The study of the isolative determination of the mixed weak bases of INAH and NA-Pas potentimetrically considering the properties of solvents for the INAH and Na-PAS, dielectric constant and solvative properties of solvents are described. The methanol: dioxan (4:1) and glacial acetic acid: dioxan (4:1) are studied first as the mixed solvent, using the N/10 perchloric acid and glacial acetic acid solution as the titrant. The authors found that there is no inflection on INAH with the methanol: dioxan solvent system and on Na-PAS at glacial acetic acid dioxan solvent system. By applying methanol glacial acetic acid dioxan (1:1:1) solvent system, Na-PAS and INAH were successfully determined isolatively from the mixed sample, showing the distinguished inflections respectively as shown in the titration curves in figures 3 and 4. It is found that this method could save considerable time for the isolative determination of the mixed sample of week bases as Na PAS and INHA which were quite difficult to be determined by the present routine at control laboratory.

• Current Optics and Photonics
• /
• 제6권3호
• /
• pp.337-343
• /
• 2022

Microfluidic chips are new devices that can manipulate liquids at the micrometer level, and terahertz (THz) time-domain spectroscopy has good applicability in biochemical detection. The combination of these two technologies can shorten the distance between sample and THz wave, reduce THz wave absorption by water, and more effectively analyze the kinetics of biochemical reactions in aqueous solutions. This study investigates the effects of different external magnetic field intensities on the THz transmission characteristics of deionized water, CuSO₄, CuCl₂, (CH₃COO)₂Cu, Na₂SO₄, NaCl, and CH₃COONa; the THz spectral intensity of the sample solutions decrease with increasing intensity of the applied magnetic field. Analysis shows that the magnetic field leads to a change in the dipole moment of water molecules in water and electrolyte solutions, which enhances not only the hydrogen-bond networking ability of water but also the hydration around ions in electrolyte solutions, increasing the number of hydrogen bonds. Increasing the intensity of this magnetic field further promotes the hydrogen-bond association between water molecules, weakening the THz transmission intensity of the solution.

• 분석과학
• /
• 제36권5호
• /
• pp.205-215
• /
• 2023

In the present study, an analytical method was proposed for detecting trifluralin in aquatic products at trace concentrations. The method employed QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) and gas chromatography coupled with tandem mass spectrometry (GC-MS/MS) as the sample preparation and measurement, respectively. The effect of the aqueous phase volume used in the QuEChERS was demonstrated, and the ratio of 10:10 (mL) between water and acetonitrile phase was used for 5 g of sample. Besides, dSPE using C18 and primary-secondary amine (PSA) was applied to remove the potential interferences from the food matrices, indicating no remarkable analyte loss. The linear range was built up from 0.50 ㎍ L^-1 to 3.0 ㎍ L^-1 (R² = 0.9993). Other criteria, i.e., repeatability (RSD_r = 0.86-1.96 %), reproducibility (RSD_R = 1.09-2.01 %), and recovery (over 90 %), were in accordance with Appendix F of AOAC (2016) for method performance. Although no trifluralin was detected for the commercial samples (fish, shrimp, and breaded shrimp), the spiked samples performed favorable recoveries and precision.

• 한국독성학회:학술대회논문집
• /
• 한국독성학회 2006년도 추계학술대회
• /
• pp.65-74
• /
• 2006

Modem drug discovery requires rapid pharmacokinetic evaluation of chemically diverse compounds for early candidate selection. This demands the development of analytical methods that offer high-throughput of samples. Naturally, liquid chromatography / tandem mass spectrometry (LC-MS/MS) is choice of the analytical method because of its superior sensitivity and selectivity. As a result of the short analysis time(typically 3-5min) by LC-MS/MS, sample preparation has become the rate- determining step in the whole analytical cycle. Consequently tremendous efforts are being made to speed up and automate this step. In a typical automated 96-well SPE(solid-phase extraction) procedure, plasma samples are transferred to the 96-well SPE plate, internal standard and aqueous buffer solutions are added and then vacuum is applied using the robotic liquid handling system. It takes only 20-90 min to process 96 samples by automated SPE and the analyst is physically occupied for only approximately 10 min. Recently, the ultra-high flow rate liquid chromatography (turbulent-flow chromatography)has sparked a huge interest for rapid and direct quantitation of drugs in plasma. There is no sample preparation except for sample aliquotting, internal standard addition and centrifugation. This type of analysis is achieved by using a small diameter column with a large particle size(30-5O ${\mu}$m) and a high flow rate, typically between 3-5 ml/min. Silica-based monolithic HPLC columns contain a novel chromatographic support in which the traditional particulate packing has been replaced with a single, continuous network (monolith) of pcrous silica. The main advantage of such a network is decreased backpressure due to macropores (2 ${\mu}$m) throughout the network. This allows high flow rates, and hence fast analyses that are unattainable with traditional particulate columns. The reduction of particle diameter in HPLC results in increased column efficiency. use of small particles (<2 urn), however, requires p.essu.es beyond the traditional 6,000 psi of conventional pumping devices. Instrumental development in recent years has resulted in pumping devices capable of handling the requirements of columns packed with small particles. The staggered parallel HPLC system consists of four fully independent binary HPLC pumps, a modified auto sampler, and a series of switching and selector valves all controlled by a single computer program. The system improves sample throughput without sacrificing chromatographic separation or data quality. Sample throughput can be increased nearly four-fold without requiring significant changes in current analytical procedures. The process of Bioanalytical Method Validation is required by the FDA to assess and verify the performance of a chronlatographic method prior to its application in sample analysis. The validation should address the selectivity, linearity, accuracy, precision and stability of the method. This presentation will provide all overview of the work required to accomplish a full validation and show how a chromatographic method is suitable for toxirokinetic sample analysis. A liquid chromatography/tandem mass spectrometry (LC-MS/MS) method developed to quantitate drug levels in dog plasma will be used as an example of tile process.

• Journal of Applied Biological Chemistry
• /
• 제57권1호
• /
• pp.83-87
• /
• 2014

신선편이 파프리카의 이산화염소수와 푸마르산의 병합 살균 처리의 효과와 그에 따른 미생물의 생장 변화를 분석하였다. 병합처리를 통해 파프리카에서의 총 호기성 세균과 접종된 L. monocytogenes는 대조구에 비해 각각 0.82, 1.21 log CFU/g의 감균 효과를 얻었다. 또한 저장 10일 후에는 미생물 수가 1.21, 2.10 log CFU/g 감소하였다. 파프리카 시료를 10일간 저장하면서 미생물 수를 측정한 결과를 Gompertz model을 이용하여 최대성장속도와 유도기를 구함으로써 미생물의 생장 예측 모델에 적용하였다. 모델 식의 적합성 평가를 위해 $R^2$, $A_f$, $B_f$, 등의 값을 계산한 결과, 모두 1에 가까운 결과가 나와 측정값과 예측된 값 사이의 적합성이 뛰어났다. 따라서 본 연구결과는 이산화염소수와 푸마르산의 병합처리는 신선편이 파프리카에 오염된 미생물 수를 감소시킬 뿐 만 아니라, 미생물의 최대성장속도를 감소시키고 유도기를 증가시킴으로써 미생물 생육을 제어할 수 있음을 보여준다.

• KSBB Journal
• /
• 제11권4호
• /
• pp.420-430
• /
• 1996

열처리된 Salmonella typhimurium 항원을 모델 분석물질로 선택하여 단지 시료만을 첨가함으로써 측정을 수행할 수 있는 1단계 immuno--chromatogra phy 분석시스템이 개발되었다. 개발된 시스템은 분 석물질 특정항체(감지항체)-gold 중합체가 건조된 상태로 축적된 glass fiber membrane(하단), 분석 물질의 다른 epltope를 인지하는 항체(포획항체)와 항 감지항체 특정항체들이 공간적으로 분리되어 고정화된 nitrocellulose membrane(중단) 그리고 흡수대로 선택된 cellulose membrane ( 상단)들로 구성된다. 이와 같은 구성성분들은 분석물질을 포함한 시료수용액이 모세관현상에 의해 연속적으로 이동되도록 부분척으로 포개어 배열되었다. 분석시스템의 성능을 조절하는 변수들은 포획항체의 농도 및 membrane 상의 고정화 위치, membrane 표면처리 와 시료운반용액에 샤용된 비반응성 단백질의 종류, 그리고 중합체의 농도로써 확인되었다. 최적조건하 에서, 시스템의 하부로부터 시료수용액을 흡수 후 15분 이내에 포획항체가 고정화된 membrane 상의 지역에 샌드위치 형상의 항원 항체 면역결합체가 형성되었고 이로부터 발생된 발색신호는 분석물질의 농도에 비례하는 것으로 나타났다. 분석물질의 측정 하한농도는 $1{\times}106$ Salmonella cells/mL인 것으로 나타났다.