• 한국의학물리학회:학술대회논문집
• /
• 한국의학물리학회 2002년도 Proceedings
• /
• pp.161-163
• /
• 2002

The BNCT(Boron Neutron Capture Therapy) facility has been developed in Hanaro(High-flux Advanced Neutron Application Reactor), a research reactor of Korea Atomic Energy Research Institute. A typical tangenial beam port is utilized with this BNCT facility. Thermal neutrons can be penetrated within the limits of the possible maximum instead of being filtered fast neutrons and gamma rays as much as possible using the silicon and bismuth single crystals. In addition to, the liquid nitrogen (LN$_2$) is used to cool down the silicon and bismuth single crystals for the increase of the penetrated thermal neutron flux. Neutron beams for BNCT are shielded using the water shutter. The water shutter was designed and manufactured not to interfere with any other subsystem of Hanaro when the BNCT facility is operated. Also, it is replaced with conventional beam port plug in order to cut off helium gas leakage in the beam port. A circular collimator, composed of $\^$6/Li$_2$CO$_3$ and polyethylene compounds, is installed at the irradiation position. The measured neutron flux with 24 MW reactor power using the Au-198 activation analysis method is 8.3${\times}$10$\^$8/ n/cm$^2$ s at the collimator, exit point of neutron beams. Flatness of neutron beams is proven to ${\pm}$ 6.8% at 97 mm collimator. According to the result of acceptance tests of the water shutter, the filling time of water is about 190 seconds and drainage time of it is about 270 seconds. The radiation leakages in the irradiation room are analyzed to near the background level for neutron and 12 mSv/hr in the maximum for gamma by using BF$_3$ proportional counter and GM counter respectively. Therefore, it is verified that the neutron beams from BNCT facility in Hanaro will be enough to utilize for the purpose of clinical and pre-clinical experiment.

• 생약학회지
• /
• 제39권3호
• /
• pp.199-202
• /
• 2008

A high performance liquid chromatographic (HPLC) method for the simultaneous determination of hesperidin and glycyrrhizin was established for the quality control of traditional herbal medicinal preparation, Pyungwi-san (PWS). 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 230 nm. The presence of hesperidin and glycyrrhizin in this extract was ascertained by retention time, spiking with each authentic standard and UV spectrum. All four compounds showed good linearity $(r^2>0.995)$ in a relatively wide concentration ranges. The R.S.D. for intra-day and inter-day precision was less than 7.0% and the limits of detection (LOD) were less than 60 ng. The mean recovery of each compound was 99.0-105.6% with R.S.D. values less than 4.0%. This method was successfully applied to the determination of contents of hesperidin and glycyrrhizin in three commercial products of PWS. These results suggest that the developed HPLC method is simple, effective and could be readily utilized as a quality control method for commercial PWS products.

• 한국임상약학회지
• /
• 제16권1호
• /
• pp.23-27
• /
• 2006

Doxorubicin (DXR) is a type of anti-cancer drug called an 'anthracycline glycoside', It works by impairing DNA synthesis, a crucial feature of cell division, and thus is able to target rapidly dividing cells. Doxorubicin is a very serious anti-cancer medication with definite potential to do great harm as well as great good. A liquid chromatography-tandem mass spectroscopy (LC-MS/MS) method was developed to identify and quantify DXR in small-volume biological samples. After the addition of internal standard (IS, $5{\mu}L\;of\;1{\mu}M/ml$ daunorubicin methanol solution) into the serum sample, the drug and IS were extracted by methanol. Following vortex for a 1min and centrifugation at 15,000g for 10 min the organic phase was transferred and evaporated under a vacuum. The residue was reconstituted with $350{\mu}L$ of mobile phase and $10{\mu}L$ was injected into C18 column with mobile phase composed of 0.05M ammonium acetate (0.1 M acetic acid adjusted to pH 3.5) and acetonitrile (40:60, v/v). The flow rate was kept constant at $350{\mu}L/min$. The ions were quantified in the multiple reaction mode (MRM), using positive ions, on a triple quadrupole mass spectrometer. The lower limits of quantification for Doxorubicin in plasma and small tissues were approximately 0.5 ng/mL and 0.5 ng/mL respectively. Intra- and inter-assay accuracy (% of nominal concentration) and precision (% CV) for all analytes were within 15%, respectively.

• Journal of Radiation Protection and Research
• /
• 제20권4호
• /
• pp.237-243
• /
• 1995

파라핀 왁스를 사용하여 건조된 농축폐액을 고화시킬 경우, 방사선적 가수분해에 의해 발생할 가능성이 있는 수소가스의 발생량을 추정하여 보았다 분석결과에 의하면, 코발트 60의 방사선 에너지에 의해 방사선적 가수분해가 주로 발생함을 알 수 있다. 200리터 드럼중 120 리터가 파라핀으로 채워졌다고 가정할 때 수소가스 발생은 초기에 $4.4{\times}10^2cm^3yr^1$이고 100년이 경과한 후는 $7.2cm^3yr^1$로 줄어든다. 수소에 의한 발화점을 25년이 경과한 후 도발할 가능성이 있으나, 폭발한계에는 1000년 이내에 도달할 가능성이 없다. 안전성 관련 주요 한계점에 도달하는 시기는 드럼내 파라핀 왁스의 채움 정도에 매우 민감하게 영향을 받는다 드럼내 공간의 감소시, 발화점에 도달 시간이 줄어듬을 알 수 있다.

• Asian Pacific Journal of Cancer Prevention
• /
• 제16권14호
• /
• pp.5987-5991
• /
• 2015

Our previous study detected aflatoxins in red chili peppers from Chile, Bolivia, and Peru, each of which have a high incidence of gallbladder cancer (GBC). Since the aflatoxin B1 concentration was not so high in these peppers, it is important to clarify the presence of other mycotoxins. Here we attempted to determine any associations between the concentrations of aflatoxins and ochratoxin A (OTA) in red chili peppers, and the corresponding GBC incidences. We collected red chili peppers from three areas in Peru: Trujillo (a high GBC incidence area), Cusco (an intermediate GBC incidence area), and Lima (a low GBC incidence rate), and from Chile and Bolivia. Aflatoxins and OTA were extracted with organic solvents. The concentrations of aflatoxins B1, B2, G1, and G2, and OTA were measured by high-performance liquid chromatography. The values obtained were compared with the incidence of GBC in each area or country. All of the red chili peppers from the three areas showed contamination with aflatoxins below the Commission of the European Communities (EC) recommended limits ($5{\mu}g/kg$), but the OTA contamination of two samples was above the EC recommended limit ($15{\mu}g/kg$). The mean concentrations of OTA in the peppers from Chile (mean $355{\mu}g/kg$, range < $5-1,059{\mu}g/kg$) and Bolivia (mean $207{\mu}g/kg$, range $0.8-628{\mu}g/kg$), which has a high incidence of GBC, were higher than that in Peru ($14{\mu}g/kg$, range < $5-47{\mu}g/kg$), which has an intermediate GBC incidence. The OTA contamination in the red chili peppers from Chile, Bolivia, and Peru was stronger than that of aflatoxins. Our data suggest that OTA in red chili peppers may be associated with the development of GBC.

• 분석과학
• /
• 제8권2호
• /
• pp.215-220
• /
• 1995

흰쥐 뇌의 선조체로부터 catecholamine, indoleamine 및 대사산물을 동시분석할 수 있는 간편한 방법을 제시하였다. 기기는 ECD를 장착한 HPLC를 사용하였고, 고정상인 $C_{18}$ 컬럼에서, 이 동상은 10mM citric acid, 0.13mM $Na_4EDTA$, 0.58mM SOS를 함유하는 35mM sodium acetate buffer(pH 3.4) : MeOH=85:15가 최적이었다. 이 때 컬럼온도는 $30^{\circ}C$였다. 이 조건으로 dopamine(DA), 3, 4-dihydroxyphenyl acetic acid(DOPAC), homovanilic acid(HVA), 5-hydroxyindole acetic acid(5-HIAA), serotonin(5-HT) 및 noradrenaline(NA)을 미량까지 분석할 수 있었고, 검출한계는 각 성분에 대해 1회 주입당 2~10pg이었다. 이 방법으로 흰쥐의 주령 및 성별에 따른 선조 체내 생체아민과 대사산물의 함량을 비교하였다. 7주령 쥐에서 암컷은 수컷보다 DA와 5-HT의 함량이 유의성 있게 높은 것으로 나타났으며, 주령이 증가함에 따라 암컷에서 DOPAC의 함량이 유의적으로 증가하였다.

• 농약과학회지
• /
• 제11권1호
• /
• pp.27-31
• /
• 2007

HPLC에 의한 배추 중 trifloxystrobin의 회수율은 $84.6{\sim}95.3%$이었고 대사산물인 CGA321113의 회수율은 $86.4{\sim}87.3%$이었으며, 검출한계는 모두 0.04 mg $kg^{-1}$이었다. 경엽처리시 배추 중 trifloxystrobin 잔류량은 수확 5일과 6일전 2회 처리, 수확 3일과 7일전 3회 처리에서 모두 농약잔류허용기준(temporary MRL, 0.5 mg $kg^{-1}$)을 초과하였다. 관주처리 배추에서의 trifloxystrobin 잔류량은 기준량(1500배 희석액 주당 150 mL) 및 배량(1500배 희석액 주당 300 mL)처리에서 각각 0.16, 0.31 mg $kg^{-1}$으로 MRL 미만이었다. 따라서 살균제 trifloxystrobin(22% 액상수화제)를 사용하여 배추 재배시 농약잔류허용기준에 의하여 토양처리가 안전할 것으로 사료되며 경엽처리시 안전사용기준으로 부적합하다고 판단된다.

• 농약과학회지
• /
• 제14권1호
• /
• pp.37-48
• /
• 2010

HPLC-UVD/MS를 이용하여 농산물 중 diacylhydrazine계 살충제인 methoxyfenozide, chromafenozide 및 tebufenozide의 잔류 분석법을 확립하였으며, 대상 농산물은 현미, 콩, 사과, 배추 및 고추를 선정하였다. 시료에 acetone을 가하여 추출된 methoxyfenozide, chromafenozide 및 tebufenozide 성분을 dichloromethane 분배법과 florisil 흡착 크로마토그래피법으로 정제하여 HPLC-UVD/MS 분석대상 시료로 하였다. 대상 농약의 동시분석을 위한 최적 HPLC 분석조건을 확립하였으며, 분석대상 농약의 분석정량한계(MQL)는 0.04 mg/kg 이었다. 각 대표 농산물에 대해 정량한계의 10 및 50배 수준에서 회수율을 검정한 결과 모든 처리농도에서 89.0~104.8% 수준을 나타내었으며, 반복 간 변이계수(CV)는 최대 3.9%를 나타내어 잔류분석 기준인 회수율 70~120% 및 분석오차 10%이내를 충족시키는 만족한 결과를 도출하였다. 본 연구에서 확립된 diacylhydrazine계 살충제인 methoxyfenozide, chromafenozide 및 tebufenozide의 HPLC-UVD 분석법은 검출한계, 회수율 및 분석오차 면에서 국제적 분석기준을 만족할 뿐만 아니라, LC/MS SIM을 이용한 분석법 또한 회수율이 우수하여 확인 및 정량법으로 사용가능한 방법이었다.

• 대한수의학회지
• /
• 제36권3호
• /
• pp.541-550
• /
• 1996

Tetracycline antibiotics have been widely used not only therapeutics but feed additives. There are many methods for the isolation and determination of tetracycline antibiotics in animal muscle tissue. But those methods take much time and labor, so it is difficult to analyse many samples simultaneously. A rapid isolation method and liquid chromatographic determination of tetracycline antibiotics in animal muscle tissue (bovine, porcine, chicken) is presented. Blank control and tetracyclines fortified samples (0.5g) were blended with $C_{18}$ containing 0.05g each of oxalic acid and disodium ethylenediaminetetraacetate. After homogenize, homogenate was transferred to glass column made from 10ml glass syringe and compressed to 4~4.5ml volume. A column made from the $C_{18}$/meat matrix was washed with hexane (8ml) and dichloromethane (8ml, if needed), following which the tetracyclines were eluted,vith methanol or 0.01M methanolic oxalic acid (8ml). The eluates containing tetracyclines analytes were free from interfering compounds when analysed by HPLC with UV detection (photodiode array at 360nm). Standard curve for each tetracycline showed a linear response at the range of $0.05{\sim}1.0{\mu}g/ml$ and tetracycline antibiotics were eluted within 4ml of eluted volume. All tetracycline antibiotics except tetracycline were stable during the concentration process at $40^{\circ}C$ and time required for concentration was 3~4 hours. Fortified samples containing oxalic aicd and EDTA represented more good recoveries than those of not-contained sample. Recoveries were 91.8~110.1% (oxytetracycline; OTC), 57.7~79.5% (tetracycline; TC), 78.1~88.6% (chlortetracyclines; CTC) and 88.4~100.6% (doxycycline; DC) in pork tissue, 101.1~126.8% (OTC), 66.4~75.4% (TC), 79.2~88.1% (CTC) and 69.3~86.7% (DC) in beef tissue, and 90.8~95.6% (OTC), 66.2~84.4% (TC), 75.7~77.2% (CTC) and 55.6~80.7% (DC) in chicken muscle tissue. The detection limits validated in muscle tissue by this method were $0.05{\mu}g/g$ for OTC and TC, and $0.1{\mu}g/g$ for CTC and DC.

• 한국환경농학회지
• /
• 제39권3호
• /
• pp.246-252
• /
• 2020

BACKGROUND: Pesticides are broadly used to control weeds and pests, and the residues remaining in crops are managed in accordance with the MRLs (maximum residue limits). Therefore, an analytical method is required to quantify the residues, and we conducted a series of analyses to select and validate the quick and simple analytical method for tolpyralate in five agricultural products using QuEChERS (quick, easy, cheap, effective, rugged and safe) method and LC-MS/MS (liquid chromatography-tandem mass spectrometry). METHODS AND RESULTS: The agricultural samples were extracted with acetonitrile followed by addition of anhydrous magnesium sulfate, sodium chloride, disodium hydrogencitrate sesquihydrate and trisodium citrate dihydrate. After shaking and centrifugation, purification was performed with d-SPE (dispersive-solid phase extraction) sorbents. To validate the optimized method, its selectivity, linearity, LOD (limit of detection), LOQ (limit of quantitation), accuracy, repeatability, and reproducibility from the inter-laboratory analyses were considered. LOQ of the analytical method was 0.01 mg/kg at five agricultural products and the linearity of matrix-matched calibration were good at seven concentration levels, from 0.0025 to 0.25 mg/L (R²≥0.9980). Mean recoveries at three spiking levels (n=5) were in the range of 85.2~112.4% with associated relative standard deviation values less than 6.2%, and the coefficient of variation between the two laboratories was also below 13%. All optimized results were validated according to the criteria ranges requested in the Codex Alimentarius Commission (CAC) and Ministry of Food and Drug Safety (MFDS) guidelines. CONCLUSION: In conclusion, we suggest that the selected and validated method could serve as a basic data for detecting tolpyralate residue in imported and domestic agricultural products.