• 제목/요약/키워드: phase sensitive detector

검색결과 54건 처리시간 0.018초

Discrimination of Ginseng Habitat by Using Instrumental Analysis Techniques

  • Sohn H. J.;Lee S. K.;Cho B. G.;Kim S. J.;Lee N. Y.;Choi D. S.;Jeong M. S.;Bae H. R.;Yang J. W.
    • 고려인삼학회:학술대회논문집
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    • 고려인삼학회 2002년도 학술대회지
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    • pp.238-252
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    • 2002
  • In order to screen out indicators for the discrimination of ginseng habitat, some physical and chemical characteristics of Korean red ginsengs (94 kinds) and Chinese red ginsengs (50 kinds) were analyzed by using a rheometer, an electronic nose system, a combined technique of solid phase micro-extraction (SPME) and gas chromatograph equipped with an electron capture detector (GC/ECD), an X-ray fluorescence spectrometer (XRF), an inductively coupled plasma mass spectrometer (ICP/MS), a near infrared spectrometer (NIRs) and high performance liquid chromatography equipped with evaporative light scattering detector (HPLC/ELSD). The results are summarized as follows: (i) The rhizome strengths of Korean red ginsengs were significantly higher than those of Chinese red ginsengs. (ii) The electronic nose patterns of Korean red ginsengs were significantly different from those of Chinese red ginsengs. (iii) Some unidentified peaks were detected not in the headspace of Korean red ginsengs but in the headspace of Chinese red ginsengs when the headspace volatiles prepared by the SPME technique were analyzed by GC/ECD. (iv) Either the content ratios of K to Ca or Mn to Fe were significantly different between Korean red ginsengs and Chinese red ginsengs. (v) The reflectance ratios of NIRs wavenumbers such as $904\;cm^{-1}\;to\;1088\;cm^{-1}$ for Korean red ginsengs were significantly different from those for Chinese red ginsengs. (vi) The content ratios of ginsenoside-Rg to ginsenoside-Re of Korean red ginsengs were significantly higher than those of Chinese red ginsengs. These results indicate that the rhizome strength, the electronic nose pattern, the occurrence of ECD-sensitive headspace volatile components, the content ratios of K to Ca and Mn to Fe, the NIRs pattern and the content ratio of ginsenoside-Rg to -Re may be indicators for the discrimination of ginseng habitat.

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GC/AED를 이용한 의료용 액화혼합가스 중 산화에틸렌 및 프레온 가스류의 몰분율 측정 (Determination of the mole fractions of ethylene oxide and freons in medical liquefied gas mixture by GC/AED)

  • 김현주;김달호;임아랑;이택홍;김진석
    • 분석과학
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    • 제25권6호
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    • pp.382-387
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    • 2012
  • 산화에틸렌($C_2H_4O$, Ethylene oxide, EtO)은 에탄올아민 같은 공업적으로 중요한 물질이나 에틸렌 글리콜의 생산 원료 또는 살균제로 이용되는 물질이다. 산화에틸렌은 불화탄화수소를 분사제 또는 바탕가스로 하여 액화혼합가스로 제조되어 열에 약한 의료기기나 저장시설의 소독에 널리 사용되고 있다. 액화혼합가스의 생산 및 사용 시 품질관리 및 안전관리를 위해 각 성분의 몰분율을 정확히 측정할 필요가 있다. 휘발성 액체시료 중 각 기체성분들은 증기압이나 끓는점 등과 같이 물리 화학적 성질이 다르므로 몰분율 측정 시 실린더 내부의 상층에 평형을 이루고 있는 기체시료 또는 하층의 기화되지 않은 액체시료를 직접 측정기기에 주입하는 방법에 따라 측정 결과가 다를 수 있다. 본 연구에서는 액화혼합가스를 액체 또는 기체 상태로 주입할 수 있는 새로운 온라인 시료도입장치를 고안하고 GC/AED (gas chromatograph-atomic emission detector)를 사용하여 산화에틸렌과 불화탄화수소 액화혼합가스를 측정하였으며 AED의 검출특성, 기기에 주입 시 시료의 상태, 측정파장에 따른 측정결과의 정확성 및 반복성을 조사하였다.

공간주파수대역에서 기저대역 확장을 통한 원전 대비시험편과 대비 보정 시험편의 초음파 영상 개선 (Ultrasonic Images Enhancement of the SS Reference Specimen and the Reference Calibration Block for NPPs by the Combining Bases of Support for Spatial Frequency)

  • 박치승;김선진
    • 한국재료학회지
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    • 제13권10호
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    • pp.651-657
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    • 2003
  • Ultrasonic microscope has been used to detect the defects on surface or inner solid. Conventionally, it has used at a single operating frequency. The resolution and quality of the measured images are determined by a characteristic of the transducer of the ultrasonic microscope. The conventional ultrasonic microscope has been used envelope detector to detect the amplitude of reflected signal, but the changes in amplitude is not sensitive enough for specimen with microstructure that in phase. In this paper, we have studied multi-frequency depth resolution enhancement with ultrasonic reflection microscope for the reflectors of a stainless steel reference specimen and a reference calibration block to be used as the material in nuclear power plants for ISI, PSI. Increased depth resolution can be obtained by taking two, three-dimensional images at more that one frequency and numerically combining the results. As results of the experiment, we could get enhanced images with the rate of contrast in proportion and high quality signal distribution for the image to the changing rate of depth for the reflectors of the two kinds of specimens.

환경시료로부터 미량 페놀류의 분석을 위한 isoButoxycarbonyl 유도체화 분석방법 적용 및 최적화 (Application and Optimization of the IsoButoxycarbonyl Derivatization method to the Analysis of Trace Level Phenols in Environmental Samples)

  • 김협;홍종기;김용화;김경례
    • Environmental Analysis Health and Toxicology
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    • 제17권1호
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    • pp.37-51
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    • 2002
  • Eleven phenols including two chlorophenols, eight alkylphenols and bisphenol A were derivatized with isobutylchloroformate to form their isobutoxycarbonyl derivatives. Standard phenol mixture was concentrated for the isobutoxycarbonyl (isoBOC) derivatization and analysed by gas chromatography/mass spectrometry (GC/MS). The recoveries of the derivatization method of alkylphenols, chlorophenols, and bisphenol A were calculated by gas chromatography/mass spectrometry-selected ion monitoring mode using two work-up methods for comparison; shaking and heating method. The linear detector responses were obtained in the concentration range of 5∼400 ng, with correlation coefficients varying from 0.9755∼0.9981. Recoveries of the alkylphenols, chlorophenols, and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring mode using two work-up methods for comparison ; the US-EPA method and the isoBOC derivatization method, Eleven phenols in water samples were extracted with dichloromethane and then concentrated. Also, solid-phase extraction (SPE) with XAD-4 and subsequent conversion to isobutoxycarbonyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The recoveries were 85.1∼109.9% and 90.3∼126.6% for the US-EPA method and the isoBOC.

한국인에서의 경구용 클로나제팜의 약물동력학적 특성 (Pharmacokinetic Characteristics of Oral Clonazepam in Korean)

  • 정지훈;유대식;박준홍;이석용;손의동
    • 약학회지
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    • 제48권5호
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    • pp.278-284
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    • 2004
  • In order to determine the bioavailability of c1onazepam, an anxiolytic drug, a simple, rapid and sensitive HPLC analysis was developed in healthy Korean volunteers. The analysis system was validated in specificity, accuracy, precision and linearity. The analysis condition we established was 2.58 min and 5 ng/$m\ell$ in retention time and limit of quantitation of c1onazepam, respectively, using reverse-phase C18 column connected to UV detector. Quantitation was performed at 235 nm wave length with p-hydroxybenzoic acid ethyl ester as internal standard. The method involved a simple extraction. In order to study blood level profiles as a function of time, eight volunteers were enrolled and orally took 6 mg clonazepam once. The blood samples were collected from 0 to 120 h after the drug administration. Mean AUC and Cmax value were 1028.17$\pm$568.165 (ng/$m\ell$$.$hr) and 41.25$\pm$10.82 (ng/$m\ell$), respectively. And mean Tmax and T$_{1}$2/ value were 1.08$\pm$0.42 (hr) and 30.78$\pm$3.26 (hr). From the results we determine the pharmacokinetic characteristics of clonazepam in Korean people using a newly developed and useful HPLC method.

HPLC법에 의한 1,2-디아미노-4,5-메틸렌디옥시벤젠을 형광유도체화제로 한 혈청 및 뇨 중의 ${\alpha}$-케토산의 분석 (Determination of ${\alpha}-Keto$ Acids in Serum and Urine Using 1,2-Diamino-4,5-methylendioxybenzene as a Fluorescent Derivatizating Agent by High Performance Liquid Chromatography)

  • 옥치완;김대기;박송자;박종세
    • 약학회지
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    • 제36권4호
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    • pp.370-378
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    • 1992
  • A simple and sensitive high performance liquid chromatographic method to quantitate ${\alpha}-keto$ acids in serum and urine was investigated. ${\alpha}-Keto$ acids react with 1,2-diamino-4,5-methylenedioxybenzene (DMB) in the presence of 2-mercapto-ethanol and sodium hydrogen sulfite to form highly fluorescent derivatives, substituted 6,7-methylenedioxyquinoxalinol. The derivatization procedure was performed in water bath at $100^{\circ}C$, and completed within 50 min. By the use of a reversed-phase column and multi-step gradient with two solvents, a mixture containing twelve of these derivatives were efficiently resolved within 35 minutes. The optimal wavelengh of the fluorescence detector are ${\lambda}_{ex}=364\;nm$ and ${\lambda}_{em}=445\;nm$. The quantitation of the individual ${\alpha}-Keto$ acids was reproducible with relative standard deviation of $3.0{\sim}7.9%$ and had a detection limits of $10{\sim}60$ fmol, except for p-hydroxyphenylpyruvic acid (960 fmol).

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2차원 Magnetic Fluxgate센서의 구현에 관한 연구 (A Study on the Implementation of the 2-Dimension Magnetic Fluxgate Sensor)

  • 박용우;김남호;류지구
    • 센서학회지
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    • 제11권2호
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    • pp.67-76
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    • 2002
  • 본 연구에서는 페라이트 링 코어를 이용한 2차원 fluxgate 센서를 제안하였으며, 본 fluxgate 센서 시스템은 2차원 자장을 측정할 수 있는 센서와 그 센서를 구동하기 위한 구동회로, 그리고 신호처리회로 등으로 구성하였다. 신호 검출 방법으로는 우수고조파 성분 검출을 위해 PSD(phase sensitivity detector) 회로를 사용하였으며, 기존의 제 2고조파 검출법과 비교하기 위해서 pick-up 코일 출력전압의 제 2고조파 성분을 FFT 스펙트럼 분석기를 사용하여 측정하였고, 이렇게 측정된 제 2고조파 성분의 전압과 PSD 단의 출력전압을 비교하였다. 그 결과 여자전류의 증가에 따라 센서의 출력전압도 증가하였으며, 구동주파수에 따른 PSD 단의 출력전압은 주파수가 1.5[kHz]일 때까지는 증가하였지만, 그 이상의 주파수에서는 감소함을 보였다. 그리고 pick-up 코일의 제 2고조파 성분의 전압은 계속 증가함을 보였다. 센서의 최대감도는 구동주파수 1.5 [kHz], 구동전류 2 [App]에서 최대값을 보였으며 감도는 약 1580 [V/T]였다. 센서의 비선형계수는 3 [G] 이내에서 제 2고조파 성분의 전압인 경우 약 1 [%]이내였으며, PSD 단 이후는 약 2.3 [%]이내였다. 그리고 각도오차는 약 ${\pm}2$ [%/FS]이내였다.

UPLC-DAD를 이용한 불환금정기산의 다성분 동시분석법 개발 (Development of an UPLC-DAD Method for Simultaneous Analysis of Eight Marker Compounds of Bulhwangeumjeonggi-san)

  • 이경희;라미차네 라마칸타;서르마 디박 쿠마르;판데야 프라카스 라즈;김세건;정현주
    • 생약학회지
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    • 제47권4호
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    • pp.366-373
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    • 2016
  • Bulhwangeumjeonggisan (BHGJGS) is a traditional herbal formulation generally used in the treatment of cold and gastritis. BHGJGS consists of eight herbal plants; Atractylodis Rhizoma, Magnoliae Cortex, Citri Pericarpium, Glycyrrhizae Radix, Agastachis Herba, Pinelliae Rhizoma, Zingiberis Rhizoma and Zizyphi Fructus. Complete standardization of this formulation has not been done yet. So, a simple and accurate method was developed and validated using Ultra Performance Liquid Chromatography (UPLC) with Diode Array Detector (DAD) for the standardization of BHGJGS. UPLC conditions were optimized using a c18 RP-Amide column with mobile phase; 0.1% phosphate buffer and acetonitrile, detection wavelength; 210 and 325 nm. The linearities of calibration curves were acceptable ($R^2$>0.9994), and the limit of detection and quantification were within the ranges of 0.011-0.091 and $0.034-0.277{\mu}g/ml$ respectively. The relative standard deviation (RSD) of intra- and inter-day precisions were under 3.61%. The RSD of repeatability was under 0.68 %. The results of recovery test were 94.4-107.9%, and the RSD were under 4.6%. The developed method was used to find the contents of standard constituents in BHGJGS mix extract powder, and two commercial formulation (A and B). The data show that the developed method was specific, sensitive, accurate, and precise for analysis of BHGJGS components.

인체 혈장 중 나돌올의 HPLC 분석법 검증 및 단회투여 후 약물동태 연구 (Validation of and HPLC Method for Nadolol in Human Plasma and Evaluation of Its Pharmacokinetics after a Single-dose in Korean Volunteers)

  • 강춘모;트란트룽;김경호;명자혜;황성주;김미영;구효정
    • Journal of Pharmaceutical Investigation
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    • 제35권6호
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    • pp.431-436
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    • 2005
  • A high-performance liquid chromatographic method was validated for quantitation of nadolol in human plasma. Nadolol and internal standard, pindolol, were extracted with tert-butyl methyl ether after addition of 10 M sodium hydroxide solution. The analytes were separated on a reverse phased C18 column using a mobile phase consisting of 0.05 M ammonium phosphate monobasic buffer, acetonitrile and methanol (81: 17:2 v/v/v) and detected using a fluorescence detector (excitation wavelength 230 nm, emission wavelength 294 nm). The method was specific and sensitive enough to detect as low as 3 ng/mL of nadolol in human plasma. Linear calibration range was 3-150 ng/mL with correlation coefficient greater than 0.999. The overall accuracy was in the range of 96.8 to 103% and precision C.V.(%) 7.30 to 12.2%. The recovery was approximately 100% and stability was confirmed during storage and sample preparation. The present HPLC method was successfully applied to study bioavailability after oral administration of 80 mg of nadolol in healthy Korean subjects. The mean $AUC_{t}$ was $1968{\pm}397\;ng{\cdot}hr/mL$ and $C_{max}$ of $186{\pm}79.3\;ng/mL$ was reached at $3.5{\pm}0.76\;hr$. The mean $t_{1/2}$ of nadolol was $17.3{\pm}2.59\;hr$.

Bioequivalence Assessment of Acephyll® Capsule to Surfolase® Capsule (Acebrophylline HCl 100 mg) by Liquid Chromatography Tandem Mass Spectrometry

  • Nam, Kyung-Don;Seo, Ji-Hyung;Yim, Sung-Vin;Lee, Kyung-Tae
    • Journal of Pharmaceutical Investigation
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    • 제41권5호
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    • pp.309-315
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    • 2011
  • A sensitive and specific liquid chromatographic method coupled with tandem mass spectrometry (LC-MS/MS) was developed for the analysis of ambroxol (active moiety of acebrophylline). After acetonitrile precipitation of proteins from plasma samples, ambroxol and the domperidone (internal standard, IS) were eluted on a C18 column. The isocratic mobile phase was consisted of 10 mM ammonium acetate and methanol (10 : 90, v/v), with flow rate at 0.2 mL/min. A tandem mass spectrometer, as detector, was used for quantitative analysis in positive mode by a multiple reaction monitoring mode to monitor the m/z 379.2${\rightarrow}$264.0 and the m/z 426.2${\rightarrow}$175.1 transitions for ambroxol and the IS, respectively. Twenty four healthy Korean male subjects received two capsules (100 mg ${\times}$ 2) of either the test or the reference formulation of acebrophylline HCl in a 2 ${\times}$ 2 crossover study, this was followed by a 1week washout period between either formulation. $AUC_{0-t}$ (the area under the plasma concentration-time curve) was calculated by the linear trapezoidal rule. $C_{max}$ (maximum plasma drug concentration) and $T_{max}$ (time to reach $C_{max}$) were compiled from the plasma concentration-time data. The 90% confidence intervals for the log transformed data were acceptable range of log 0.8 to log 1.25 (e.g., log 0.8964 - log 0.9910 for $AUC_{0-t}$ log 0.8690 - log 1.0750 for $C_{max}$). The major parameters, $AUC_{0-t}$ and $C_{max}$ met the criteria of Korea Food and Drug Administration for bioequivalence indicating that Acephyll$^{(R)}$ capsule (test) is bioequivalent to Surfolase$^{(R)}$ capsule (reference).