• 제목/요약/키워드: liquid-solid phase separation

검색결과 74건 처리시간 0.023초

HgCdTe를 이용한 Infrared Detector의 제조와 특성 (Fabrication and Its Characteristics of HgCdTe Infrared Detector)

  • 김재묵;서상희;이희철;한석룡
    • 한국군사과학기술학회지
    • /
    • 제1권1호
    • /
    • pp.227-237
    • /
    • 1998
  • HgCdTe Is the most versatile material for the developing infrared devices. Not like III-V compound semiconductors or silicon-based photo-detecting materials, HgCdTe has unique characteristics such as adjustable bandgap, very high electron mobility, and large difference between electron and hole mobilities. Many research groups have been interested in this material since early 70's, but mainly due to its thermodynamic difficulties for preparing materials, no single growth technique is appreciated as a standard growth technique in this research field. Solid state recrystallization(SSR), travelling heater method(THM), and Bridgman growth are major techniques used to grow bulk HgCdTe material. Materials with high quality and purity can be grown using these bulk growth techniques, however, due to the large separation between solidus and liquidus line on the phase diagram, it is very difficult to grow large materials with minimun defects. Various epitaxial growth techniques were adopted to get large area HgCdTe and among them liquid phase epitaxy(LPE), metal organic chemical vapor deposition(MOCVD), and molecular beam epitaxy(MBE) are most frequently used techniques. There are also various types of photo-detectors utilizing HgCdTe materials, and photovoltaic and photoconductive devices are most interested types of detectors up to these days. For the larger may detectors, photovoltaic devices have some advantages over power-requiring photoconductive devices. In this paper we reported the main results on the HgCdTe growing and characterization including LPE and MOCVD, device fabrication and its characteristics such as single element and linear array($8{\times}1$ PC, $128{\times}1$ PV and 4120{\times}1$ PC). Also we included the results of the dewar manufacturing, assembling, and optical and environmental test of the detectors.

  • PDF

Method for Screening and Confirming Meldonium in Human Urine by High-Resolution Mass Spectrometry and Identification of Endogenous Interferences for Anti-Doping Testing

  • Kim, Yongseok;Jeong, Dawon;Min, Hophil;Sung, Changmin;Park, Ju-hyung;Son, Junghyun;Lee, Kang Mi;Kim, Ho Jun;Lee, Jaeick;Kwon, Oh-Seung;Kim, Ki Hun
    • Mass Spectrometry Letters
    • /
    • 제8권2호
    • /
    • pp.39-43
    • /
    • 2017
  • Meldonium is a drug for treating ischemia by expanding the arteries but it can also enhance the performance of sports players. The World Anti-Doping Agency (WADA) has included it in the list of prohibited substances since 2016. Meldonium is one of the challenging substances for anti-doping testing because it is difficult to recover by general liquid-liquid or solid phase extraction due to its permanent charge and high polarity. Therefore, high-performance liquid chromatography (HPLC) is currently used by injecting a diluted urine sample (known as the "dilute-and-shoot" strategy). There is no loss of target compounds in the extraction/cleanup procedure but its high matrix effect could interfere in their separation or detection from the endogenous urinary compounds. We report a single method using high-resolution mass spectrometry that can be used for both screening and confirmation, which follows the "dilute-and-shoot" strategy. In this method, the endogenous compounds' interfering peaks in the mass spectrum are separated at a high resolution of FWHM 140,000, and the results are suitable for substance detection following the WADA guidelines. The interferences in the obtained mass spectrum of the urine matrix are identified as acetylcholine, lysine, and glutamine by further analysis and database searching. Validation of the method is performed in routine anti-doping testing, and the limit of detection is 50 ng/mL. This method uses simple sample preparation and a general reverse phase HPLC column, and it can be easily applied to other substances.

LC-MS/MS를 이용한 퇴비 및 액비 중 항생제 동시 분석법 개발 (Development of Simultaneous Analytical Method of Veterinary Antibiotics in Manure using Liquid Chromatography Coupled with Tandem Mass Spectrometry)

  • 정형석;이영준;이한솔;;;박병준;김장억;심재한
    • 한국환경농학회지
    • /
    • 제36권3호
    • /
    • pp.201-210
    • /
    • 2017
  • 전국의 퇴비 및 액비 시료에서 대상 항생제 종9 (ceftiofur, clopidol, florfenicol, sulfamethazine, sulfamethoxazole, sulfathiazole, tetracycline, tiamulin, tylosin)을 pH 6 McIlvaine buffer를 사용하여 아세트산 함유 아세토니트릴, $Na_2Cit.5H_2O$, $Na_3Cit.2H_2O$로 추출 후 $C_{18}$과 PSA로 정제하여 LC-MS/MS로 분석하는 모니터링을 수행하였다. 그 중 5종의 항생제 sulfamethazine, sulfathiazole, tylosin, tiamulin 및 clopidol이 국내 퇴액비 시료에서 검출되었으며 제안한 분석법은 퇴 액비 중 잔류 항생제 모니터링을 위한 빠르고 간편한 시험법이라 사료 된다. 본 실험을 통하여 퇴비 및 액비 중 축산 항생제의 잔류 현황을 파악하여 모니터링 자료를 확보하였고 이를 활용하여 검출된 항생제들이 안전한 토양 및 생태 환경 유지 및 관리의 기초 자료와 더불어 환경기준 예비 항목 및 설정(안)을 위한 기초자료로 제공 및 다양하게 활용될 수 있을 것으로 판단된다.

효소적으로 합성된 대칭형과 비대칭형 Triacylglycerol 혼합물의 In Vitro Digestion에서의 소화율 비교 (Comparison of Hydrolysis from In Vitro Digestion Using Symmetric and Asymmetric Triacylglycerol Compounds by Enzymatic Interesterification)

  • 우정민;이기택
    • 한국식품영양과학회지
    • /
    • 제43권6호
    • /
    • pp.842-853
    • /
    • 2014
  • 본 연구는 고올레산 해바라기유(high oleic sunflower oil, HOSO), palmitic ethyl ester 및 stearic ethyl ester를 이용하여 대칭형 유지와 비대칭형 유지를 합성하였으며, 이를 이용하여 in vitro digestion에서의 소화율(%)을 비교하고자 하였다. 생성된 대칭형 유지와 비대칭형 유지는 acetone을 이용하여 분별함으로써 대칭형 유지는 I, II, III으로, 비대칭형 유지는 IV, V로 분별되었다. 그 후 분별물들을 이용하여 in vitro digestion을 진행함으로써 소화율(%)과 농도변화량(mg/mL/min)을 비교하였으며, 분별물들의 위치별 지방산 및 TAG 조성 분석, DSC를 통한 흡열 및 발열곡선 분석, solid fat index와 융점 측정을 통해 특성을 알아보고자 하였다. 위치별 지방산 조성 분석 결과 I, II, III은 sn-2 위치에 palmitic acid와 stearic acid의 합이 4.9~6.5 area%로 나타나 주로 대칭형 TAG로 이루어졌고, IV와 V는 41.9~43.9 area%로 나타나 주로 비대칭형 TAG로 구성되어 있는 것으로 확인되었다. 한편 in vitro digestion을 진행하여 분별물간의 가수분해율(%)을 비교한 결과, 반응시간 120분에서는 V만 다른 분별물에 비해 약 40% 정도 소화가 되지 않았으며, V의 융점이 $49^{\circ}C$로 반응온도($37^{\circ}C$)보다 높았다. 초기 반응시간(15분)에서는 I,II>IV>III>V 순으로 소화가 되지 않았으며, 각 분별물에서 ${\bigcirc}{\bigcirc}{\bigcirc}$와 POS/PSO의 가수분해율(%)을 비교해 본 결과 TAG 간의 가수분해율 차이가 없는 것으로 나타났다. 한편 III과 IV를 비교해 보았을 때, IV가 III에 비해 두 개의 포화지방산으로 구성된 TAG 함량이 약 40 area% 적지만 complete melting point가 III과 유사한 것으로 나타나 비대칭형 TAG가 대칭형 TAG에 비해 융점이 높다는 것을 알 수 있었다. 따라서 slip melting point가 in vitro digestion 결과에 가장 큰 영향을 미치며, 융점은 총지방산 조성에서의 포화지방산 함량이 높을수록, 두 개의 포화지방산으로 구성된 TAG의 함량이 높을수록, 비대칭형 TAG로 이루어질수록 높아짐을 알 수 있었다.

Full validation of high-throughput bioanalytical method for the new drug in plasma by LC-MS/MS and its applicability to toxicokinetic analysis

  • Han, Sang-Beom
    • 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.

  • PDF

LC-MS/MS를 이용한 농경지 토양 중 항생제 모니터링 (Monitoring of Veterinary Antibiotics in Agricultural Soils using Liquid Chromatography Coupled with Tandem Mass Spectrometry)

  • 이영준;최정희;정형석;이한솔;박병준;김장억;심재한
    • 한국환경농학회지
    • /
    • 제35권3호
    • /
    • pp.166-174
    • /
    • 2016
  • 농경지 토양에서 대상항생제 6종(amoxicillin, ampicillin, chlortetracycline, enrofloxacin, oxytetracycline, tetracycline을 아세트산 함유 아세토니트릴, Na2Cit.5H2O, Na3Cit.2H2O과 Na2-EDTA로 추출 후 C18으로 정제하여 LC-MS/MS로 분석하는 모니터링을 수행하였다. 그 중 2종의 항생제, chlortetracycline과 enrofloxacin이 국내 농경지 토양에서 검출되었다. 제안한 분석법은 토양 중 잔류 항생제 모니터링을 위한 빠르고 간편한 시험법이었고 다양한 활용이 가능할 것으로 보인다.

LC/MS/MS를 이용한 산화성 스트레스 지표로써 소변 중 8-iso-PGF 분석 (Determination of 8-iso-PGF as Oxidative Stress Marker in Human Urine by High Performance Liquid Chromatography with Tandem Mass Spectrometry)

  • 고영림;이은희;채홍재;최경호;백도명
    • 한국환경보건학회지
    • /
    • 제36권1호
    • /
    • pp.44-51
    • /
    • 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.

공기중 이소시아네이트류의 측정 및 분석방법에 관한 비교연구 (A Comparison of Sampling and Analytical Methods for Airborne Isocyanates)

  • 변혜정;윤충식;백남원
    • 한국환경보건학회지
    • /
    • 제22권2호
    • /
    • pp.32-42
    • /
    • 1996
  • This study was performed to evaluate accuracy and precision of filter method and impinger method for analyzin airborne isocyanates in mixture (2, 6-TDI, HDI, 2, 4-TDI, MDI). Filter method was performed using the OSHA Method 42 and impinger method using the NIOSH Method 5521. The samples were analyzed by high performance liquid chromatography-ultraviolet detector (HPLC-UVD). After the optimum operating conditions for each method were investigated, samples with various concentration levels were quantified at the conditions. The precision was expressed by the pooled coefficient of variation(C.V.) and the accuracy by overall accuracy. The results are summarized as follows: 1. The optimum condition of filter method was determined at 35/65 ACN/buffer (0.01 M ammonium acetate) in mobile phase. And in case of impinger method, it was at 30/70 ACN/buffer(0.2 M sodium acetate). The effect of concentrations of acetate on the separation of the peaks was not significant, but, the effect of ACN/buffer ratio was significant. 2. The correlation coefficients for the two methods were above 0.9 in all isocyanate compounds. Average recovery efficiencies for 2, 6-TDI, HDI, 2, 4-TDI and MDI in filter method were 92.4%, 102.6%, 87.3% and 101.0%, respectively. Those in impinger method were 106.6%, 106.7%, 99.0% and 103.6%, respectively. As a result, the recovery efficiency of impinger method was higher than those of filter method in analyzing isocyanate compounds. 3. The pooled coefficients of variations of the methods were slightly higher than expected. The overall accuracies of the methods were within $\pm 25%$ for each isocyanate compound. Since these results satisfy NIOSH criteria, the accuracy of the experiment is appropriate. 4. As seen above, impinger method is more efficient than filter method. But, there are many disadvantages in impinger method. Therefore, solid sorbent such as a glass fiber filter must be developed in order to have the high efficiency not less than that of impinger method in the future.

  • PDF

LC-MS/MS를 이용한 해수 및 수산용수 중 플루오로퀴놀론계 항생제 동시 분석법 정립 (Simultaneous Analysis of Prohibited Antibiotics (Fluoroquinolones) in Seawater and Effluents Released by Aquaculture Using LC-MS/MS)

  • 이미경;이인석;최민규;이성규;이원찬
    • 한국수산과학회지
    • /
    • 제56권4호
    • /
    • pp.428-437
    • /
    • 2023
  • A simultaneous analytical method was developed and validated for the analysis of prohibited fluoroquinolone (FQ) antibiotics including norfloxacin, ofloxacin, and pefloxacin, released by aquaculture in seawater and effluents. The samples were filtered, and extracts were obtained using a solid phase extraction cartridge with methanol (MeOH). The extracts were concentrated, and analyzed using ultra-performance liquid chromatography-tandem mass spectrometry. Two different columns and four different mobile phases were compared to achieve optimal separation and sensitivity for target compounds. Typical validation parameters including linearity, recovery of surrogate standard, instrument detection limit (IDL), limit of quantification (LOQ), and method detection limit (MDL) were evaluated. The linearity of calibration curves was over 0.999. Recoveries of surrogate ranged from 87.6% to 113%. The LOQ of target compounds was approximately 3-8 times lower than those reported in previous studies. The IDL and MDL were 0.06-0.57 and 0.06-0.37 ng/L, respectively. Seven effluent samples collected from an aquaculture located in Jeju were analyzed; however, not all target compounds were detected in the samples, suggesting that the banned antibiotics were not used. Overall, this established method was able to simultaneously analyze the three FQ antibiotics, and may be useful for monitoring prohibited antibiotics in the fishery industry.

Simultaneous determination of illegal galactagogue adulterants in supplement diets by LC-MS/MS

  • Lee, Ji Hyun;Cho, So-Hyun;Park, Han Na;Park, Hyoung Joon;Kim, Nam Sook;Park, Sung Kwan;Kang, Hoil
    • 분석과학
    • /
    • 제31권4호
    • /
    • pp.171-178
    • /
    • 2018
  • Recently, for successful lactation, many breastfeeding mothers seek various products, including herbal medicine, dietary supplements, and prescribed medicines, to improve milk production. As demand for galactogogues grows, it is highly possible that pharmaceutical galactogogues may be adulterated with illegal products to maximize their efficacy. For continuous control and supervision of illegal products, we developed and validated a simple and sensitive LC-MS/MS method capable of simultaneously determining five galactogogues. Chromatographic separation was conducted using an Agilent Poroshell $120SB-C_{18}$ column with a mobile phase consisting of 20 mM ammonium formate (pH 5.4) and 100 % acetonitrile. The total run time was 13 min per analyte. The proposed method was performed according to the guidelines of the International Conference of Harmonization and it produced reliable results. This method showed high sensitivity and specificity, with a limit of detection (LOD) and limit of quantitation (LOQ) of 0.01-0.82 ng/mL and 0.02-2.45 ng/mL, respectively, for the solid- and liquid-type samples. Specificity was evaluated by analyzing matrix-blank samples spiked with the target compounds at LOQ levels, which provided a good separation of all peaks without interference. Additionally, the repeatability and intermediate precision were typically <15 %, whereas the recovery was 80-120 % of the values obtained using blank samples. Thus, we concluded that this method could be used for the identification and quantification of galactogogues in food or herbal products.