• 제목/요약/키워드: Limit Of Stability

검색결과 1,065건 처리시간 0.031초

LC-MS/MS를 이용한 농산물 중 Fluoroimide의 잔류농약 분석법 개선 (Improvement of an Analytical Method for Fluoroimide Residue in Agricultural Products Using LC-MS/MS)

  • 김남영;박은지;심재한;이정미;정용현;오재호
    • 한국식품위생안전성학회지
    • /
    • 제36권3호
    • /
    • pp.220-227
    • /
    • 2021
  • Fluoroimide는 감과 감자의 둥근무늬낙엽병과 역병을 억제하는데 효과가있는 살진균제로서, 이전 사용되었던 fluoroimide의 시험법은 전처리시 발암물질인 benzene을 사용하는 문제가 있었으며, 복잡한 시험법으로 인해 시간이 오래걸리고 효율이 떨어지는 단점이 있었다. 또한, fluoroimide의 특성상 산성에서 안정한 편이므로 전처리 시 이를 고려해야 하는 문제가 있었으며, PLS시행에 따라 기존의 정량한계인 0.05 mg/kg보다 낮은 정량한계 요구로 인해 fluoroimide에 대한 새로운 전처리방법이 필요하였다. Fluoroimide가 산성에서 안정한 특성을 고려하여, 추출 시 4N의 염산을 사용하였고 용매는 acetic acid가 포함된 acetonitrile을 사용하였으며, MgSO4와 NaCl을 통해 추출하였다. 정제는 C18 (Octadecylsilane)과 GCB (graphitized carbon black)를 첨가하여 정제하였으며, 기기분석은 LC-MS/MS로 분석하였다. 대표농산물 5종(현미, 감자, 대두, 감귤, 고추)을 대상으로 정량한계(0.01 mg/kg), 정량한계 10배(0.1 mg/kg), 정량한계 50배(0.5 mg/kg)의 수준으로 회수율 실험을 5반복 실시하였으며, 그 결과는 농산물 5종에서 85.7-106.9%의 회수율을 확인하였으며, 분석오차는 15.6% 이하의 결과를 보여, 국제식품 규격위원회 가이드라인의 잔류농약 분석 기준 및 '식품등 시험법 마련 표준절차에 관한 가이드라인(2016)'에 부합하였다. 상기의 결과를 통해 개선한 fluoroimide의 시험법은 benzene을 대체해 실험자의 안전성을 확보하였고, QuEChERS법을 적용하여 효율을 높여, 안전관리에 대한 공정시험법으로서 활용가능할 것으로 사료된다.

Effects of Neutral Particle Beam on Nano-Crystalline Silicon Thin Film Deposited by Using Neutral Beam Assisted Chemical Vapor Deposition at Room Temperature

  • Lee, Dong-Hyeok;Jang, Jin-Nyoung;So, Hyun-Wook;Yoo, Suk-Jae;Lee, Bon-Ju;Hong, Mun-Pyo
    • 한국진공학회:학술대회논문집
    • /
    • 한국진공학회 2012년도 제43회 하계 정기 학술대회 초록집
    • /
    • pp.254-255
    • /
    • 2012
  • Interest in nano-crystalline silicon (nc-Si) thin films has been growing because of their favorable processing conditions for certain electronic devices. In particular, there has been an increase in the use of nc-Si thin films in photovoltaics for large solar cell panels and in thin film transistors for large flat panel displays. One of the most important material properties for these device applications is the macroscopic charge-carrier mobility. Hydrogenated amorphous silicon (a-Si:H) or nc-Si is a basic material in thin film transistors (TFTs). However, a-Si:H based devices have low carrier mobility and bias instability due to their metastable properties. The large number of trap sites and incomplete hydrogen passivation of a-Si:H film produce limited carrier transport. The basic electrical properties, including the carrier mobility and stability, of nc-Si TFTs might be superior to those of a-Si:H thin film. However, typical nc-Si thin films tend to have mobilities similar to a-Si films, although changes in the processing conditions can enhance the mobility. In polycrystalline silicon (poly-Si) thin films, the performance of the devices is strongly influenced by the boundaries between neighboring crystalline grains. These grain boundaries limit the conductance of macroscopic regions comprised of multiple grains. In much of the work on poly-Si thin films, it was shown that the performance of TFTs was largely determined by the number and location of the grain boundaries within the channel. Hence, efforts were made to reduce the total number of grain boundaries by increasing the average grain size. However, even a small number of grain boundaries can significantly reduce the macroscopic charge carrier mobility. The nano-crystalline or polymorphous-Si development for TFT and solar cells have been employed to compensate for disadvantage inherent to a-Si and micro-crystalline silicon (${\mu}$-Si). Recently, a novel process for deposition of nano-crystralline silicon (nc-Si) thin films at room temperature was developed using neutral beam assisted chemical vapor deposition (NBaCVD) with a neutral particle beam (NPB) source, which controls the energy of incident neutral particles in the range of 1~300 eV in order to enhance the atomic activation and crystalline of thin films at room temperature. In previous our experiments, we verified favorable properties of nc-Si thin films for certain electronic devices. During the formation of the nc-Si thin films by the NBaCVD with various process conditions, NPB energy directly controlled by the reflector bias and effectively increased crystal fraction (~80%) by uniformly distributed nc grains with 3~10 nm size. The more resent work on nc-Si thin film transistors (TFT) was done. We identified the performance of nc-Si TFT active channeal layers. The dependence of the performance of nc-Si TFT on the primary process parameters is explored. Raman, FT-IR and transmission electron microscope (TEM) were used to study the microstructures and the crystalline volume fraction of nc-Si films. The electric properties were investigated on Cr/SiO2/nc-Si metal-oxide-semiconductor (MOS) capacitors.

  • PDF

테르페나딘 체내동태 연구를 위한 혈청 중 펙소페나딘의 HPLC 정량법 개발 및 검증 (Development and Validation of an HPLC Method for the Pharmacokinetic Study of Fexofenadine in Human)

  • 조혜영;강현아;김윤균;최후균;이용복
    • Journal of Pharmaceutical Investigation
    • /
    • 제35권6호
    • /
    • pp.437-443
    • /
    • 2005
  • A rapid, selective and sensitive reversed-phase HPLC method for the determination of a major metabolite of terfenadine, fexofenadine, in human serum was developed, validated, and applied to the pharmacokinetic study of terfenadine. Fexofenadine and internal standard, haloperidol were extracted from human serum by liquid-liquid extraction with acetonitrile and analyzed on a $Symmetry^{TM}$ C8 column with the mobile phase of 1% triethylamine phosphate (pH 3.7)-acetonitrile (67:33, v/v, adjusted to pH 5.6 with triethylamine). Detection wavelength of 230 nm for excitation, 280 nm for emission and flow rate of 1.0 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^{3}$ factorial design using a fixed fexofenadine concentration (50 ng/mL) with respect to its peak area and retention time. In addition, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 10-500 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of serum was 10 ng/mL, which was sensitive enough for the pharmacokinetic studies of terfenadine. The overall accuracy of the quality control samples ranged from 95.70 to 114.58% for fexofenadine with overall precision (% C.V.) being 3.53-14.39%. The relative mean recovery of fexofenadine for human serum was 90.17%. Stability studies (freeze-thaw, short-term, extracted serum sample and stock solution) showed that fexofenadine was stable during storage, or during the assay procedure in human serum. However, the storage at $-70^{\circ}C$ for 4 weeks showed that fexofenadine was not stable. The peak area and retention time of fexofenadine were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of fexofenadine in human serum samples for the pharmacokinetic studies of orally administered Tafedine tablet (60 mg as terfenadine) at three different laboratories, demonstrating the suitability of the method.

Inflammatory Effect of Light-Emitting Diodes Curing Light Irradiation on Raw264.7 Macrophage

  • Jeong, Moon-Jin;Kil, Ki-Sung;Lee, Myoung-Hwa;Lee, Seung-Yeon;Lee, Hye-Jin;Lim, Do-Seon;Jeong, Soon-Jeong
    • 치위생과학회지
    • /
    • 제19권2호
    • /
    • pp.133-140
    • /
    • 2019
  • Background: The light-emitting diode (LED) curing light used is presumed to be safe. However, the scientific basis for this is unclear, and the safety of LED curing light is still controversial. The purpose of this study was to investigate the effect of LED curing light irradiation according to the conditions applied for the polymerization of composite resins in dental clinic on the cell viability and inflammatory response in Raw264.7 macrophages and to confirm the stability of LED curing light. Methods: Cell viability and cell morphology of Raw264.7 macrophages treated with 100 ng/ml of lipopolysaccharide (LPS) or/and LED curing light with a wavelength of 440~490 nm for 20 seconds were confirmed by methylthiazolydiphenyl-tetrazolium bromide assay and microscopic observation. The production of nitric oxide (NO) and prostaglandin $E_2$ ($PGE_2$) was confirmed by NO assay and $PGE_2$ enzyme-linked immunosorbent assay kit. Expression of interleukin $(IL)-1{\beta}$ and tumor necrosis factor $(TNF)-{\alpha}$ in total RNA and protein was confirmed by reverse transcription polymerase chain reaction and Western blot analysis. Results: The LED curing light did not affect the viability and morphology of normal Raw264.7 cells but affected the cell viability and induced cytotoxicity in the inflammation-induced Raw264.7 cells by LPS. The irradiation of the LED curing light did not progress to the inflammatory state in the inflammation-induced Raw264.7 macrophage. However, LED curing light irradiation in normal Raw264.7 cells induced an increase in NO and $PGE_2$ production and mRNA and protein expression of $(IL)-1{\beta}$ and $(TNF)-{\alpha}$, indicating that it is possible to induce the inflammatory state. Conclusion: The irradiation of LED curing light in RAW264.7 macrophage may induce an excessive inflammatory reaction and damage oral tissues. Therefore, it is necessary to limit the long-term irradiation which is inappropriate when applying LED curing light in a dental clinic.

디피리다몰 체내동태 연구를 위한 혈청 중 디피리다몰의 HPLC 정량법 개발 및 검증 (Development and Validation of an HPLC Method for the Pharmacokinetic Study of Dipyridamole in Human)

  • 조혜영;강현아;문재동;최후균;이용복
    • Journal of Pharmaceutical Investigation
    • /
    • 제36권1호
    • /
    • pp.45-51
    • /
    • 2006
  • A rapid, selective and sensitive reversed-phase HPLC method for the determination of dipyridamole in human serum was developed, validated, and applied to the pharmacokinetic study of dipyridamole. Dipyridamole and internal standard, loxapine, were extracted from human serum by liquid-liquid extraction with diethyl ether and analyzed on a Nova Pak $C_{I8}$ column with the mobile phase of 40 mM ammonium acetate:methanol:acetonitrile (35:35:30)(v/v/v, pH 7.8). Detection wavelength of 280 nm and flow rate of 1.0 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^3$ factorial design using a fixed dipyridamole concentration (50 ng/mL) with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 2-2000 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of serum was 2 ng/mL, which was sensitive enough for pharmacokinetic studies of dipyridamole. The overall accuracy of the quality control samples ranged from 103.94 to 105.86% for dipyridamole with overall precision (% C.V.) being 4.60-11.49%. The relative mean recovery of dipyridamole for human serum was 97.64%. Stability studies showed that dipyridamole was stable during storage, or during the assay procedure in human serum. The peak area and retention time of dipyridamole were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of dipyridamole in human serum samples for the pharmacokinetic studies of orally administered Dimor tablet (75 mg as dipyridamole) at three different laboratories, demonstrating the suitability of the method.

염산프로메타진 체내동태 연구를 위한 혈청 중 프로메타진의 HPLC 정량법 개발 및 검증 (Development and Validation of HPLC Method for Pharmacokinetic Study of Promethazine in Human)

  • 조혜영;강현아;이화정;최후균;이용복
    • Journal of Pharmaceutical Investigation
    • /
    • 제36권1호
    • /
    • pp.23-29
    • /
    • 2006
  • A rapid, selective and sensitive reversed-phase HPLC method for the determination of promethazine in human serum was developed, validated, and applied to the pharmacokinetic study of promethazine. Promethazine and internal standard, chlorpromazine, were extracted from human serum by liquid-liquid extraction with n-hexane containing 0.8% isopropanol and analyzed on a Capcell Pak CN column with the mobile phase of acetonitrile-0.2 M potassium dihydrogen phosphate (42:58, v/v, adjusted to pH 6.0 with 1 M NaOH). Detection wavelength of 251 nm and flow rate of 0.9 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^{3}$ factorial design using a fixed promethazine concentration (10 ng/mL) with respect to its peak area and retention time. In addition, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 1-40 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 1 mL of serum was 1 ng/mL, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the quality control samples ranged from 96.15 to 105.40% for promethazine with overall precision (% C.V.) being 6.70-11.22%. The relative mean recovery of promethazine for human serum was 63.54%. Stability (freeze-thaw and short-term) studies showed that promethazine was stable during storage, or during the assay procedure in human serum. However, the storage at $-80^{\circ}C$ for 4 weeks showed that promethazine was not stable. Extracted serum sample and stock solution were not allowed to stand at ambient temperature for 12 hr prior to injection. The peak area and retention time of promethazine were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of promethazine in human serum samples for the pharmacokinetic studies of orally administered Himazin tablet (25 mg as promethazine hydrochloride) at three different laboratories, demonstrating the suitability of the method.

에토돌락 체내동태 연구를 위한 혈청 중 에토돌락의 HPLC 정량법 개발 및 검증 (Development and Validation of an HPLC Method for the Pharmacokinetic Study of Etodolac in Human)

  • 조혜영;강현아;문재동;최후균;이용복
    • Journal of Pharmaceutical Investigation
    • /
    • 제35권4호
    • /
    • pp.265-271
    • /
    • 2005
  • A rapid, selective and sensitive reversed-phase HPLC method for the determination of etodolac in human serum was developed, validated, and applied to the pharmacokinetic study of etodolac. Etodolac and internal standard, ibuprofen were extracted from human serum by liquid-liquid extraction with hexane/isopropanol (95:5, v/v) and analyzed on a Luna C18(2) column with the mobile phase of 1% aqueous acetic acid-acetonitrile (4:6, v/v). Detection wavelength of 227 nm and flow rate of 1.0 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^3$ factorial design using a fixed etodolac concentration $(1\;{\mu}g/mL)$ with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of $0.05-40\;{\mu}g/mL$ with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of serum was 0.05 ${\mu}g/mL$, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the quality control samples ranged from 92.00 to 110.00% for etodolac with overall precision (% C.V.) being 1.08-10.11%. The percent recovery for human serum was in the range of 76.73-115.30%. Stability studies showed that etodolac was stable during storage, or during the assay procedure in human serum. The peak area and retention time of etodolac were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of etodolac in human serum samples for the pharmacokinetic studies of orally administered Lodin XL tablet (400 mg as etodolac) at three different laboratories, demonstrating the suitability of the method.

페노프로펜 체내동태 연구를 위한 혈청 중 페노프로펜의 HPLC 정량법 개발 및 검증 (Development and Validation of an HPLC Method for the Pharmacokinetic Study of Fenoprofen in Human)

  • 조혜영;강현아;김윤균;사홍기;이용복
    • Journal of Pharmaceutical Investigation
    • /
    • 제35권6호
    • /
    • pp.423-429
    • /
    • 2005
  • A selective and sensitive reversed-phase HPLC method for the determination of fenoprofen in human serum was developed, validated, and applied to the pharmacokinetic study of fenoprofen calcium. Fenoprofen and internal standard, ketoprofen, were extracted from human serum by liquid-liquid extraction with diethyl ether and analyzed on a Luna C18(2) column with the mobile phase of acetonitrile-3 mM potassium dihydrogen phosphate (32:68, v/v, adjusted to pH 6.6 with phosphoric acid). Detection wavelength of 272 nm and flow rate of 0.25 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^{3}$ factorial design using a fixed fenoprofen concentration $(2\;{\mu}g/mL)$ with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of $0.05-100\;{\mu}g/mL$ with correlation coefficients greater than 0.999. The lower limit of quantification using 1 mL of serum was $0.05\;{\mu}g/mL$, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the quality control samples ranged from 92.27 to 109.20% for fenoprofen with overall precision (% C.V.) being 5.51-11.71 %. The relative mean recovery of fenoprofen for human serum was 81.7%. Stability (freeze-thaw, short and long-term) studies showed that fenoprofen was not stable during storage. But, extracted serum sample and stock solution were allowed to stand at ambient temperature for 12 hr prior to injection without affecting the quantification. The peak area and retention time of fenoprofen were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of fenoprofen in human serum samples for the pharmacokinetic studies of orally administered Fenopron tablet (600 mg as fenoprofen) at three different laboratories, demonstrating the suitability of the method.

체내동태 연구를 위한 혈청 중 펜톡시필린의 HPLC 정량법 개발 및 검증 (Development and Validation of an HPLC Method for the Pharmacokinetic Study of Pentoxifylline in Human Serum)

  • 조혜영;강현아;류희두;이화정;문재동;이용복
    • Journal of Pharmaceutical Investigation
    • /
    • 제36권2호
    • /
    • pp.89-95
    • /
    • 2006
  • A selective and sensitive reversed-phase HPLC method for the determination of pentoxifylline in human serum was developed, validated, and applied to the pharmacokinetic study of pentoxifylline. Pentoxifylline and internal standard, chloramphenicol, were extracted from the serum by liquid-liquid extraction with dichloromethane and analyzed on a Luna CI8(2) column with the mobile phase of acetonitrile-0.034 M phosphoric acid (25:75, v/v, adjusted to pH 4.0 with 10 M NaOH). Detection wavelength of 273 nm and flow rate of 0.8 mL/min were used. This method showed linear response over the concentration range of 10-500 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of the serum was 10 ng/mL, which was sensitive enough for pharmacokinetic studies of pentoxifylline. The overall accuracy of the quality control samples ranged from 89.3 to 92.7% for pentoxifylline with overall precision (% C.V.) being 4.1-9.2%. The relative mean recovery of pentoxifylline for human serum was 105.8%. Stability (stock solution, short and long-term) studies showed that pentoxifylline was not stable during storage. But three freeze-thaw cycles and extracted serum samples were stable. This method showed good ruggedness (within 15% C.V.) and was successfully applied for the analysis of pentoxifylline in human serum samples for the pharmacokinetic studies of orally administered $Trental^{\circledR}$ tablet (400 mg pentoxifylline), demonstrating the suitability of the method.

인공습지 조성후 생물다양성 증진 효과에 관한 연구 -서울공고 생태연못을 중심으로- (The Effects of the Biodiversity Increase after Creation of the Artificial Wetland -The Case of Ecological Pond at Seoul Technical High School-)

  • 김귀곤;조동길
    • 한국조경학회지
    • /
    • 제27권3호
    • /
    • pp.1-17
    • /
    • 1999
  • The purpose of this study is to evaluate the creation techniques of artificial wetland, one of biotopes developed to promote biodiversity in urban areas, and to look for improvement steps. Specifically, artificial wetland creation techniques were categorized into living environment and living creature classification. Being living conditions for creations, habitat environment was reviewed with a focus on water and soil environments. Living creatures were classified into plants, insects, fish, and birds. The evaluation of creation techniques was done in post-construction evaluation while considering the creation of habitats for living creatures. Intervention by users, changes in living environment and living species, and relevance of creation techniques were reviewed. Key results of this study are as follows. (1) Water environment for the living environment of creatures provides a suitable environment conditions for the living of creatures through a process easing the use of piped water. Various water depths and embankment appear to have a positive impact on the living of aquatic life. In particular, embankment covered in soil naturally played an important role as a place for the activities of aquatic insects and young fish as well as the growth of aquatic plants. (2) Various aquatic and ground plants to promote insect-diversity, shallow water, and old-tree logs had contributed greatly in increasing the types and number of insects. Aquatic insects. Aquatic insects were seen much particularly in areas where aquatic plants are rich but water is shallow than any other areas. (3) A space piled with stone to provide habitats for fish was not much used. However, it was observed that fish used embankment built with natural stones and embankment using logs in areas where water is deep. In addition, it was confirmed that 1,500 fish that had been released propagated using various depths and places for birth. (4) It was analyzed that techniques (creation of island, log setting, and creation of man-made bird nests) to provide habitats and to attract birds are not serving their roles. In such a case, it is believed that species had not increased due to the smallness as well as isolated features of the area. Based on theoretical review, they are judged to be areas that are likely to be used when a greater variety of birds is introduced. It is judged that attracting and keeping more birds at the site, such spaces need to be linked systematically in the future in terms of building eco-network while ensuring an adequate living areas. (5) In the study areas, users intervened greatly. As a result, a blockage was created preventing the normal growth of plants and non-indigenous plants were introduced. In order to limit the intervention by users, setting enough buffer zones, and environment education programs were urgently required. D/H=1>Hyangkyo> houses on the river>temples>lecture halls. D/H ratio of the backside areas is as follows. D/H=1>Hyangkyo>houses on the river>lecture halls. 4. Inner garden were planted deciduous than evergreen trees with Lagerstroemia indica. Enclosed dominant trees were planted by Pinus densiflora, Querces seuata. construct GEM strain, and examined for the expression and functional stability in microcosms.

  • PDF