• Journal of Korean Society on Water Environment
• /
• v.25 no.5
• /
• pp.720-726
• /
• 2009

We investigated the most effective pre-treatment processes and LC/MS/MS condition for microcystins analysis. With a step-by-step pre-treatment, efficiencies of several established methods were compared. At the level of cell burst, sonication method was found to be the most efficient. As a mycrocystins first extraction solvent, 5% acetic acid showed the highest efficiency. An isolation and recovery rate of mycrocystins of ODS Sep-Pak $C_{18}$ cartridge was higher than HLB SPE cartridge. As a final elution solvent from cartridge, 100% MeOH had a better efficiency than others. Using a LC/MS/MS, effective analytical methods were established. C18 reverse column was used and gradient elution was performed with using acetonitrile, 0.1% formic acid as a mobile phase. We analysed to 0.8 mL/min flow rate fit to the $5{\mu}m$ particle size column and $55^{\circ}C$ housing temperature. The validity of established analytical method was evaluated that MDL as average $0.050{\pm}0.014{\mu}g/L$ and LOQ as average $0.160{\pm}0.045{\mu}g/L$ had a good sensitivity over 40 magnification rather than $2{\mu}g/L$ detection limit of HPLC.

• Journal of Korean Society on Water Environment
• /
• v.26 no.3
• /
• pp.446-453
• /
• 2010

This study was investigated nine nitrosamines in small tributary rivers, sewage treatment plants (STPs) and drinking water treatment plants. They are N-nitrosodimethylamine (NDMA), N-nitrosomethylethylamine (NMEA), N-nitrosodiethylamine (NDEA), N-nitrosopyrrolidine (NPYR), N-nitrosodi-n-propylamine (NDPA), N-nitrosomorpholine (NMOR), N-nitrosopiperidine (NPIP), N-nitrosodi-n-butylamine (NDBA) and N-nitrosodiphenylamine (NDPHA). The nine nitrosamines were analyzed by gas chromatography mass spectrometry (GC/MS) using solid phase extraction (SPE) with a coconut charcoal cartridge. Among the nine nitrosamines, NDMA, NMEA, NDEA, NDPA NDBA and NDPHA were detected in small tributary rivers and sewage tretment plants. In small tributary rivers, NDMA, NMEA, NDEA, NDPA, NDBA and NDPHA were obtained as ND~16.4 ng/L, ND~17.7 ng/L, ND~102.4 ng/L, ND~455.4 ng/L, ND~330.1 ng/L and ND~161.0 ng/L, respectively. Also NDMA, NMEA, NDEA, NDPA and NDBA were investigated ND~821.4 ng/L, 22.5~55.4 ng/L, 53.2~588.5 ng/L, ND~56.6 ng/L and ND~527.9 ng/L in STPs, respectively. In drinking water treatment plants, NMEA and NDEA concentration were increased to as high as 38.8 ng/L after ozonation process. However nitrosamines were decreased subsequent biological activated carbon (BAC) treatment process. It was supposed that nitrosamines were formed by $O_3$ oxidation and were removed by biodegradation of BAC.

• Journal of Hydrogen and New Energy
• /
• v.16 no.2
• /
• pp.103-110
• /
• 2005

Proton conducting solid polymer electrolyte (SPE) membranes have been used in many energy technological applications such as water electolysis, fuel cells, redox-flow battery, and other electrochemical devices. The availability of stable membranes with good electrochemical characteristics as proton conductivity at high temperatures above 80 $^{\circ}C$ and low cost are very important for its applications. However, the presently available perfluorinated ionomers are not applicable because of high manufacturing cost and high temperature use to the decrease in the proton conductivity and mechanical strength. In order to make up for the weak points, the block copolymer (BPSf) of polysulfone and poly (phenylene sulfide sulfone) were synthesized and sulfonated. The electrolyte membranes were prepared with phosphotungstic acid (HPA)/sulfonated BPSf via solution blending. This study would be desirable to investigate the interaction between the HPA and sulfonated polysulfone. The results showed that the characteristics of SPSf/HPA blend membrane was a better than Nafion at high temperature, 100 $^{\circ}C$. These membranes proved to have a high proton conductivity, $6.29{\times}10-2$ S/cm, a water content, 23.9%, and a ion exchange capacity, 1.97 meq./g dry membrane. Moreover, some of the membranes kept their high thermal and mechanical stability.

• KOREAN JOURNAL OF CROP SCIENCE
• /
• v.35 no.6
• /
• pp.481-486
• /
• 1990

A survey was carried out on the cold-induced sterility of paddy rice in 1988 in the alpine area of Kangweon province when cold spell occurred during late July to early August, During this period minimum temperature as low as 8.5$^{\circ}C$ and 5.7$^{\circ}C$ was recorded at Dunnae and Jinbu, respectively. The rice cultivars, which encountered this cold spe]J at meiotic stage of microspore, were damaged by sterility in most alpine areas of higher than 300m in altitude. To secure spilkelet fertility higher than 80% it was estimated that the minimum and average air temperature accumulated during 13 days of meiotic stage should be higher than 2$25^{\circ}C$ and 285$^{\circ}C$, respectively and/or the duration of lower than 17$^{\circ}C$ in minimum temperature should not exceed fivedays during that period.

• Journal of Environmental Health Sciences
• /
• v.32 no.5 s.92
• /
• pp.440-445
• /
• 2006

Acetaminophen (paracetamol), generally used as a pain reducing agent, has good analgesic efficacy in toothaches and headaches, but is of little use in inflammatory and visceral pain. This study was performed to analyze the level of acetaminophen in the Kyongahn river and to investigate the ecological risks of target compounds. Sampling sites were Haesil, Soopyo, Wangsan, Kyongahn, Jiwol, Kwangdong, Paldang and they were analyzed in June and August, 2005. Acute toxicity of acetaminophen wwas evaluated for Daphnia magna. From the ecotoxicological results, environmental risk assessments were performed for acetaminophen residues in Kyongahn river to predict their potential adverse effect. Acetaminophen was detected at Kyonahn river, $0.439{\mu}g/l$). The toxic concentration of acetaminophen calculated with 48-h $LC_{50}$ values as 16.9 mg/l. These results indicated that acetaminophen had no significant ecotoxicological impact on short-term acute exposure.

• Journal of Environmental Health Sciences
• /
• v.40 no.6
• /
• pp.435-441
• /
• 2014

Objectives: Bisphenol A, or BPA, is a chemical component in polycarbonate plastic with which many people come into contact every day. A great deal of controversy has arisen over its safety since this material, which is known to disrupt the human endocrine system and cause neurological difficulties and cancer, is commonplace in beverage containers, food can liners, and receipt paper rolls. In this study, we determined the levels of exposure to BPA of workers in the service industry depending on the number of receipts contacted. Methods: The participants were 16 male and 18 female workers employed in the service industry. Using a questionnaire, we investigated general and job characteristics. Urine samples were collected and analyzed by the LC-MS/MS technique after enzymatic hydrolysis and solid phase extraction (SPE). Results: The geometric mean (GM) concentration of urinary BPA from all subjects was 1.02 ng/ml. Workers were exposed significantly to more BPA according to the number of receipts they contacted, their work experience, and working hours per day. The BPA concentration of those who touched more than 100 receipts per day was 3.09 ng/ml, while that of the other participants was 0.61 ng/ml. It was shown that wearing gloves can protect from BPA exposure. Conclusion: We determined the urinary BPA concentrations of workers in service industry and found that the contact with receipts could increase the BPA exposure of service workers.

• Korean Journal of Veterinary Service
• /
• v.28 no.3
• /
• pp.203-213
• /
• 2005

Oxytetracycline, tetracycline, chlortetracycline and doxycycline in honey were separated by solid phase extraction (SPE) and determined with high performance liquid chromatography (HPLC) with UV/Visible detector. Analysis was carried out using following conditions: XTerra $C_8$ column $(3.9\times150mm\;i.d. 5{\mu}m)$, mobile phase composed of 0.01M oxalic acid : methanol : acetonitrile (820 : 80 : 100, v/v/v), isocratic pump at a flow rate of 0.9 ml/min. and $50{\mu}l$ of injection volume, UV/Visible detector with wavelength of 360nm. The calibration curves of four tetracyclines showed linearity $(\gamma^2>0.999)$ at concentration range of $100\~1,000 ng/ml$. The recoveries in fortified honey represented more than $70\%$ with low coefficient of variation $(<10\%)$ for concentration range of four tetracyclines. The detection limits for oxytetracycline, tetracycline, chlortetracycline and doxycycline were 13.8, 14.6, 26.2 and 24.9ng/g in acacia honey. respectively. We also monitored tetracyclines residue in domestic honey [n : 38, acacia (20), wild flower (18) ] and foreign honey [n=22, legally distributed (13), illegally distributed (9)] using modified Charm II screening and HPLC confirmation methods. Seven of the 60 samples $(11.7\%)$ were suspect positive using modified Charm II screening test. Chlortetracycline residue was found in one foreign honey (illegally distributed) tested at concentrations of 0.22 ppm. Conclusively, for more effective control of tetracyclines used in beekeeping should be further survey for residues in honey and also national guidelines (maximum residue limit : MRL) and methods should be obligatory.

• Restorative Dentistry and Endodontics
• /
• v.28 no.3
• /
• pp.222-231
• /
• 2003

The purpose of this study was to compare shear bond strength and interfacial pattern of composite bond-ed to dentin using self-etching adhesive systems. Sixty extracted human molars with exposed occlusal dentin were divided into four groups and bonded with four adhesives and composites. Single Bond/Filtek Z 350(SB), Tyrian SPE-One-Step Plus/Aelitefil(TY), Prompt L-Pop/Filtek Z 250(LP), and One-Up Bond F/palfique Toughwell(OU). The results of this study were as follows; 1 Shear bond strength for OU was significantly lower than that of other groups(p＜0.05). No significant difference was founded among SB, TY, and LP. 2. Failure modes to dentin showed adhesive and mixed for SB TY and LP, but them for OU showed adhesive in all spceimens. 3. Dentin-resin interface showed close adaptation for SB, TY, and LP, but it showed gap for OU. 4. The hybrid layers for TY, LP OU were thinner than that of SB. Adhesive layers were observed between composite and hybrid layer, which were 5 $\mu\textrm{m}$ thick for TY and 10 $\mu\textrm{m}$ thick for OU.

• Proceedings of the Korean Society for Food Science of Animal Resources Conference
• /
• 2005.10a
• /
• pp.310-316
• /
• 2005

축산식품(우유)내의 잔류항생물질을 신속하고 간편하고 정확하게 분석하기 위한 시험법 개발을 목적으로 하였다. 축산식품내의 일반적인 잔류항생물질에 대한 지금까지의 분석법으로는 Bioassay법, TLC법, ELISA법, GC법 및 HPLC법 등이 있지만 Streptomycin/dihydrostreptomycin, neomycin에 대한 HPLC법은 거의 확립되어 있지 않은 실정이다. 우리나라의 공인 검사법으로는 Bioassay법 및 HPLC법등이 있지만 그러나 지금까지의 방법으로는 검출감도가 낮은 것이 큰 문제점으로 되어 왔다. 본 연구에서는 STP에 대한 HPLC법에 대한 보고한 Edder 방법 중에 clean-up 과정 및 이동상 조건을 대폭 수정하여 STP의 분리 및 검출감도를 낮추려고 시도하였다. 본 연구에 사용된 유도체화 장치 Post-Column Derivatization Instrument PCX 5100 (Pickering La-boratories, Inc.)의 컬럼 온도는 $40^{\circ}C$, 오븐온도 $55^{\circ}C$, 유도체화 용매 유속 0.6ml/min 이동상 유속 0.8ml/min으로 검출기는 형광검출기를 이용하여 STP 검출에 대해 만족할 만한 결과를 얻었다. 이때의 분석소요시간은 약 15분이었다. 표준시료 STP의 검량선은 넓은 농도범위(0.02${\sim}$1.0ppm)에서 양호한 직선성을 나타냈다. 본 시험법에 의한 검출한계는 limit of detection(LOD)은 0.02ppm이었으며, 적어도 우유에서의 MRL이 0.6ppm임을 감안하면 STP를 정량적으로 정도 좋게 측정할 수 있다는 것을 확인했다. 상기의 조건하에서 실제시료인 우유에 표준 STP를 0.5ppm을 spiking한 후 SPE상에서 SCX(Strong cation exchange column)을 통한 clean-up과정을 거친 후의 STP의 limit of quantification(LOQ)는 약 0.44ppm이었으며, 이에 대한 회수율은 89.7${\pm}$2.3%(n=6)를 나타냈다. 실제 CODEX에서 권장한 우유의 MRL이 0.6ppm인 점을 감안하면 CODEX권고치에 도달할 수 있는 것으로 판단되었다. 따라서 본 연구에서 개발 된 시험법은 지금까지 국내적으로 STP에 대한 시험법이 확립되어 있지 않은 것으로 이와 아울러 간편한 parallux와 병용해 STP에 대한 정량 및 정성 분석을 유도체화 장치 및 형광검출기를 이용해 잔류항생물질 STP에 대한 분석시험법을 개발하였다.

• Korean Journal of Veterinary Service
• /
• v.25 no.1
• /
• pp.23-29
• /
• 2002

A method was developed to separate, detect and qualify aldicarb, bendiocarb, carbaryl, carbofuran, ethiofencarb, methomyl, methiocarb, propoxur in meats and fruits. Experimental beef and fork samples were fortified with 0.05mg/kg of carbamate pesticides for analysis. Carbamate-detected pear by HPLC fluorescence detector(HPLC/FLS) are extracted with acetonitril and refined by solid phase extraction(SPE) filled with aminopropyl-bonded silca, In the following step, the injected materials into LC/MS are analyzed to result in the fact that bendiocarb, carbaryl, carbofuran, ethiofencarb, methomyl, methiocarb, propoxur presents several sorts of fraction ions following with; [M+H]$^{+}$, [M+Na]$^{+}$,［M-CONH$CH_3$]$^{+}$, [M-OCONH$CH_3$]$^{+}$. In addition, ethiofencarb presents [M-SCH$_2$$CH_3$]$^{+}$ ion distinctive and aldicarb presents [M+Na]$^{+}$ and [M-OCONH$CH_3$]$^{+}$ ion which is the most decisive fraction ion for pesticides such as bendiocarb, carbaryl, carbofuran, ethiofencarb, methiocarb, methomyl, propoxur excluding [M+H]$^{+}$ ion. However, [M-OCONH$CH_3$]$^{+}$ and [M-OCONH$CH_3$]$^{+}$ fraction ion charactering carbamate pesticides are detected most efficiently with fragment voltage 50ev. As a result, for rluantitative analysis, [M+Na]$^{+}$ ion is the most decisive ion for detection of aldicarb and [M+H]$^{+}$ ion is the most decisive fraction ion for Pesticides such as bendiocarb, carbaryl, carbofuran, ethiofencarb, methiocarb, methomyl, propoxur. Carbaryl-detected pear by HPLC/FLS are analyzed by L/MS and the result shows that [M+H]$^{+}$ and [M-CONH$CH_3$]$^{+}$ ions charactering carbaryl are detected.ering carbaryl are detected.