• Bulletin of the Korean Chemical Society
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• 제34권6호
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• pp.1783-1790
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• 2013

A simultaneous analytical method has been developed for the fluorimetric determination of haloacetonitriles (HANs) [dichloroacetonitrile (DCAN), trichloroacetonitrile (TCAN), dibromoacetonitrile (DBAN), haloacetamides [dichloroacetamide (DCAD), and trichloroacetamde (TCAD)] in drinking water by using the combined on-line perconcentration/reversed phase liquid chromatography (RPLC)-postcolumn detection system. This on-line perconcentration system was achieved by employing a precolumn packed with a commercial solid phase extraction (SPE) sorbent for the enrichment and purification of the target analytes. The haloacetonitriles and haloacetamides were separated on CN analytical column in a 7.5% methanol-0.02 M phosphate buffered mobile phase at pH 3. The column effluents were reacted with postcolumn reagents of ophthaldialdehyde (OPA) and sulfite ion at pH 11.5, to produce a highly fluorescent isoindole fluorophore, which were measured with a fluorescence detector. Under the optimized conditions for RPLC and the postcolumn derivatization system all of the coefficient of determination of the standard calibration curves for the target analytes were over 0.99 and had a linear range from 5 to 100 ${\mu}g/L$. The detection limits showed 1.6 ${\mu}g/L$ for DCAD, 0.1 ${\mu}g/L$ for TCAD, 0.6 ${\mu}g/L$ for DCAN, 1.6 ${\mu}g/L$ for TCAN and 1 ${\mu}g/L$ for DBAN, and the recoveries were ranged from 64 to 99% except for DCAD with precisions less than 4.9% in distilled water, and from 72(${\pm}4%$) to 116%(${\pm}2%$) in tap water.

• Geomechanics and Engineering
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• 제15권5호
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• pp.1091-1100
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• 2018

In this study, the relationships between hydraulic conductivity of GCLs and physico-chemical properties of bentonites were assessed. In addition to four factory manufactured GCLs, six artificially prepared GCLs (AP-GCLs) were tested. AP-GCLs were prepared in the laboratory without bonding or stitching. A total of 20 hydraulic conductivity tests were conducted using flexible wall permeameters ten of which were permeated with distilled deionized water (DIW) and the rest were permeated with tap water (TW). The hydraulic conductivity of GCLs and AP-GCLs were between $5.2{\times}10^{-10}cm/s$ and $3.0{\times}10^{-9}cm/s$. The hydraulic conductivities of all GCLs to DIW were very similar to that of GCLs to TW. Then, simple regression analyses were conducted between hydraulic conductivity and physicochemical properties of bentonite. The best correlation coefficient was achieved when hydraulic conductivity was related with clay content (R=0.85). Liquid limit and plasticity index were other independent variables that have good correlation coefficients with hydraulic conductivity (R~0.80). The correlation coefficient with swell index is less than other parameters, but still fairly good (R~0.70). In contrast, hydraulic conductivity had poor correlation coefficients with specific surface area (SSA), smectite content and cation exchange capacity (CEC) (i.e., R < 0.5). Furthermore, some post-test properties of bentonite such as final height and final water content were correlated with the hydraulic conductivity as well. The hydraulic conductivity of GCLs had fairly good correlation coefficients with either final height or final water content. However, those of AP-GCLs had poor correlations with these variables on account of fiber free characteristics.

• 대한기계학회:학술대회논문집
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• 대한기계학회 2001년도 춘계학술대회논문집E
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• pp.125-130
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• 2001

Experimental and analytical researches have been conducted on the twin-fluid atomizers for better droplet breakup during the past decades. But, the studies on the disintegration mechanism still present a great challenge to understand the drop behavior and breakup structure. In an effort to describe the aerodynamic behavior of the sprays issuing from the internal mixing counter-swirling nozzle, the spatial distribution of axial (U) radial (V) and tangential (W) components of droplet velocities are investigated across the radial distance at several axial locations of Z=30, 50, 80, 120 and 170mm, respectively. Experiments were conducted for the liquid flow rates which was kept constant at 7.95 g/s and the air injection pressures were varied from 20 kPa to 140 kPa. Counter-swirling internal mixing nozzles manufactured at angles of $15^{\circ},\;30^{\circ},\;45^{\circ}$ and $60^{\circ}$ the central axis with axi-symmetric tangential-drilled holes was considered. The distributions of velocities and turbulence intensities are comparatively analyzed. PDPA is installed to specify spray flows, which have been conducted along the axial downstream distance from the nozzle exit. Ten thousand of sampling data was collected at each point with time limits of 30 second. 3-D automatic traversing system is used to control the exact measurement. It is observed that the sprays with all swirl angle have the maximum SMD for on air injection pressure of 20 kPa and 140 kPa with centerline, respectively. The nozzle with swirl angle of $60^{\circ}$ has vest performance.

• BMB Reports
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• 제43권7호
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• pp.506-511
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• 2010

The levels of salivary cortisol and cortisone in Korean adults were measured for the first time using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The salivary cortisol and cortisone were separated within 10 min. The regression coefficients (r) of the calibration curves were greater than 0.999 for the two steroids. The limits of quantitation (LOQ) were 0.2 ng/ml for cortisol and 1 ng/ml for cortisone. The intra-day precisions of the assay were <3.9% and 8.6% for cortisol and cortisone respectively, and the inter-day precisions were <1.9% and 4.3% for cortisol and cortisone, respectively. The salivary cortisone concentrations were approximately 4-9 times higher than those of salivary cortisol during the daytime. Diurnal rhythms, during which the cortisol and cortisone concentrations were higher in the morning than in the afternoon, were also observed. The present assay may be useful for the diagnosis of several adrenal dysfunctions in clinical biochemistry.

• 한국환경보건학회지
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• 제36권2호
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• pp.155-162
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• 2010

Aflatoxin $B_1$, a known human carcinogen, is the member of aflatoxin subfamily that is most frequently found in contaminated foods. Epidemiological studies have suggested that aflatoxins may be associated with human liver cancer and acute hepatitis. Recently it was reported that the traditional medical herbs sold in domestic markets are contaminated with aflatoxins. Long-term administration of these contaminated medicines could result in adverse health effects. Therefore, it is important to evaluate the levels of exposure to aflatoxin in people who ingest traditional herbal medicines. Blood samples were collected, before and after the herbal medicine intake, from 151 subjects who visited the hospital. The metabolite of aflatoxin $B_1$ in blood, aflatoxin $B_1$-albumin (aflatoxin $B_1$-lysine), is reportedly an appropriate internal exposure indicator, and its levels in the collected bloods were therefore analyzed using a liquid chromatography-mass spectrometry. The analytical method of aflatoxin $B_1$-lysine in blood was firstly optimized in Korea and the levels were detected below quantification limits (2 pg/mg albumin) in this study population. Consequently, the exposure levels of aflatoxin $B_1$ by ingestion of herbal medicines were low but it is important to monitor routinely due to the possibility of risk on the aflatoxin exposure.

• 한국환경보건학회지
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• 제36권1호
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• pp.44-51
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• 2010

This study aimed to develop analytical method for 8-isoprostanes as biomarkers for oxidative stress with LC/MS/MS technique and to apply the method for human urine samples. Analyzed compounds for urinary oxidative stress markers were 7 stereo-isomers of prostaglandins and the internal standard (iso-$PGF_{2{\alpha}}-d_4$) was used to adjust the recovery rate. The method for determining urinary iso-$PGF_{2{\alpha}}$ consisted of solid phase extraction and LC/MS/MS detection. Separation of isomers of prostaglandins completed by porous graphitic carbon column and buffer solution. Detection limits for urinary markers of oxidative stress, iso-$PGF_{2{\alpha}}$ with LC/MS/MS were 0.01 ng/ml by S/N ratio 3 and 0.028 ng/ml by calculated as to FDA method. The recovery (92.8~101.9%) and precision (8.8~20.7%) of analysis were feasible for detecting iso-$PGF_{2{\alpha}}$ in real human urine samples. We detected 4 isomers of prostaglandins in human urine samples. Mean (standard deviation) of urinary iso-$PGF_{2{\alpha}}$ concentration were 0.231 (0.117) ng/mg creatinine for smoking group and 0.154 (0.082) ng/mg creatinine for non-smoking group.

• 대한화학회지
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• 제43권2호
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• pp.182-192
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• 1999

글로우 방전(Glow Discharge, GD)과 유도결합플라스마(Inductively Coupled Plasma, ICP)-원자 방출분광법(Atomic Emission Spectrometer, AES)에서 사용되는 새로운 장치를 개발하였다. ICP-AES에서 GDAES로 전환하는 데 불과 15분 정도 소요되기 때문에, 고체 시료 및 액체시료에 포함된 극미량 원소분석을 신속하게 수행할 수 있다. 실험변수 중에서 냉각기체 유속, 시료운반기체 유속, 절단기체 유속, 보조기체 유속, 측정깊이, 이온 통과관 크기, 그리고 rf 전원의 세기 변화에 따른 원자 방출 복사선 변화에 미치는 영향을 조사 연구하였다. Cd(I) 228.8 nm, Mn(II) 257.61 nm, and Fe(II) 259.95 nm에서 측정한 검출한계는 각각 3.86, 1.49, 5.79 ppb로 측정되었으며, 직선성은 1.000으로서 우수하였다.

• 한국식품위생안전성학회지
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• 제8권1호
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• pp.25-35
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• 1993

본 연구에서는 쇠고기, 돼지고기, 닭고기 중에 잔류하는 설파메라진(SMR), 설파메타진(SMT), 설파모노메톡신(SMMX), 설파디메톡신(SDMX), 설파퀴녹살린(SQX), 후라졸리돈(FZ), 죠렌(ZOL) , 에토파베이트 (EPB)등 합성항균제 8종에 대한 신속하고 간편한 동시분석 방법을 검토하였다. 동시분석파장으로 270nm, 이동상 용매로는 0.05M Oxalic acid : Acetonitile(22: 78), 시료 추출용매로 물과 디클로로메탄을 사용하였고 세정과정은 헥산/물. 물/디클로로메탄 분배를 이용하였다. 각 시료에 합성항균제 표준용액을 첨가하고 위의 과정을 거친 최종 추출액을 HPLCdp 주입하여 나타난 각 합성항균제의 분리는 좋았고, 각 시료에서의 대상 합성항균제들의 회수율은 쇠고기에서 74~99%, 돼지고기에서 73~99% 닭에서 75~96%로 나타났다. 검출한계는 SMR, SMT, SMMX, SDMX, EPB에서 5 ppb, SQX, FZ, ZOL에서 8ppb로 나타났으며 각 합성 항균제들의 흡수파장시험 및 pH 변화에 의한 피크분리실험에서 실제 업무수행 중에 검출된 약제를 다른 장비를 사용하지 않고 단지 HPLC만으로도 확인이 가능하였다.

• 한국식품위생안전성학회지
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• 제5권3호
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• pp.131-138
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• 1990

Aflatoxins is a chemically diverse group of toxic secondary metabolites that are produced by fungi and often occur in agricultural commodities. Because of their wide range of toxic effects, Aflatoxins cause severe economic losses to farmers and livestock producers and pose a health to human consuming contaminated foods. Long term prospects for biotechnological control of Aflatoxins require elucidation of the specific steps and regulation of their biosynthetic pathways . Aflatoxin determinations can be approached many ways. It is essential to safely handle all experimental materials associated with aflatoxin analysis or aflatoxigenic fungi Visual screening of suspect samples, base on the presence of conidial head of the aspergillus flavus group, and screening samples for the presence of bright greenish yellow flourescence are not chemical tests and such screening techniques may allow aflactoxin contaminated lots into commerce. Microcolumn screening procedures should always be used in conjunction with a quantitative method. Several thin layer chromatography(TLC) and high performance liquid chromatography(HPLC) methods are suitable for quantitation and are in general use. Immunochemical Methods such as the ELISA or affinity column chromatography methods are being rapidly developed. The chemical and immunochemical methods can be reliable if care is taken, using suitable controls and personnel that are well trained . All analytical laboratories should stress safety and include suitable analytical validation procedure. Especially a worldwide enquiry was undertaken in recent to obtain up-to-date information about aflatoxin legislation in as many countries of the world as possible. The information concerns aflatoxin in foodstuffs. aflatoxin MI in dairy products, aflatoxins in animal feedstuffs. Limits and regulations for aflatoxin have been expended in recent with more countries having legislation on subject, more products, and more aflatoxins covered by this legislation.

• Natural Product Sciences
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• 제14권3호
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• pp.147-151
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• 2008

A high performance liquid chromatographic (HPLC) method for the simultaneous determination of marker constituents, baicalin and glycyrrhizin was established for the quality control of traditional herbal medicinal preparation, Eul-Ja-Tang (EJT). Separation and quantification were successfully achieved with a Waters XTerra RP18 column ($5{\mu}m$, 4.6 mm I.D. ${\times}$ 150 mm) by gradient elution of a mixture of acetonitrile and water containing 0.03% phosphoric acid (pH 2.03) at a flow rate of 1.0 mL/min. The diode-array UV/VIS detector (DAD) was used for the detection and the wavelength for quantification was set at 250 nm. The presence of baicalin and glycyrrhizin in this decoction was ascertained by retention time, spiking with each authentic standard and UV spectrum. Both baicalin and glycyrrhizin showed good linearity ($r^2$ > 0.999) in a relatively wide concentration ranges. The R.S.D. for intra-day and inter-day precision was less than 5% and the limits of detection (LOD) were about 30 ng. The mean recovery of each compound was 99.5 - 101.2% with R.S.D. values less than 4.0%. This method was successfully applied to the determination of contents of baicalin and glycyrrhizin in three commercial products of EJT, which resulted in the difference in the contents of these compounds. These results suggest that the developed HPLC method is simple, effective and could be readily utilized as a quality control method for commercial EJT products.