• Title/Summary/Keyword: Analytical mode

Search Result 935, Processing Time 0.03 seconds

Development and validation of an LC-MS/MS method for the simultaneous analysis of 26 anti-diabetic drugs in adulterated dietary supplements and its application to a forensic sample

  • Kim, Nam Sook;Yoo, Geum Joo;Kim, Kyu Yeon;Lee, Ji Hyun;Park, Sung-Kwan;Baek, Sun Young;Kang, Hoil
    • Analytical Science and Technology
    • /
    • v.32 no.2
    • /
    • pp.35-47
    • /
    • 2019
  • In this study, high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was employed to detect 26 antidiabetic compounds in adulterated dietary supplements using a simple, selective method. The work presented herein may help prevent incidents related to food adulteration and restrict the illegal food market. The best separation was obtained on a Shiseido Capcell Pak(R) C18 MG-II ($2.0mm{\times}100mm$, $3{\mu}m$), which improved the peak shape and MS detection sensitivity of the target compounds. A gradient elution system composed of 0.1 % (v/v) formic acid in distilled water and methanol at a flow rate of 0.3 mL/min for 18 min was utilized. A triple quadrupole mass spectrometer with an electrospray ionization source operated in the positive or negative mode was employed as the detector. The developed method was validated as follows: specificity was confirmed in the multiple reaction monitoring mode using the precursor and product ion pairs. For solid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL, and for liquid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL. Satisfactory linearity was obtained from calibration curves, with $R^2$ > 0.99. Both intra and inter-day precision were less than 13.19 %. Accuracies ranged from 80.69 to 118.81 % (intra/inter-day), with a stability of less than 14.88 %. Mean recovery was found to be 80.6-119.0 % and less than 13.4 % RSD. Using the validated method, glibenclamide and pioglitazone were simultaneously determined in one capsule at concentrations of 1.52 and 0.53 mg (per capsule), respectively.

Simultaneous quantitative determination of urinary cholesterol, desmosterol and lanosterol in pravastatin treated rats by gas chromatography/mass spectrometry (Gas Chromatography/Mass Spectrometry를 이용한 Pravastatin 투여 쥐의 뇨 중 Cholesterol, Desmosterol, Lanosterol의 동시분석법)

  • Kumar, Bhowmik Salil;Chung, Bong Chul;Lee, Young-Joo;Yi, Hong Jae;Jung, Byung Hwa
    • Analytical Science and Technology
    • /
    • v.22 no.5
    • /
    • pp.407-414
    • /
    • 2009
  • A simultaneous determination method for cholesterol, lanosterol and desmosterol was developed using gas chromatography/mass spectrometry. Urine was enzymatically hydrolyzed with ${\beta}$-glucuronidase/arylsulfatase. Samples were prepared using extractions with a mixture of ethyl acetate-hexane (2:3, v/v), followed by derivatization with a mixture of MSTFA/TMSI/TMCS (100:2:5 v/v/v). All analyses were performed using GC/MS in selective ion monitoring mode. Good linearities ($r^2=0.998{\sim}0.999$) in calibration curve and a satisfactory recovery (80.0%~113%) were achieved. Accuracy and precision values within ${\pm}15%$ in the concentration range of 5 to 200 ng/mL were also observed for all compounds. The developed method was applied to pravastatin-treated (70 and 250 mg/kg/day for 7 days, oral) hyperlipidemia rats. Those sterols were significantly lower in drug-treated rats compared to the controls, which justifies the drug efficacy. Therefore, these results indicate that the developed method was successfully applied to examine statin drug efficacy with urine sample.

Prediction of the Successful Defibrillation using Hilbert-Huang Transform (Hilbert-Huang 변환을 이용한 제세동 성공 예측)

  • Jang, Yong-Gu;Jang, Seung-Jin;Hwang, Sung-Oh;Yoon, Young-Ro
    • Journal of the Institute of Electronics Engineers of Korea SC
    • /
    • v.44 no.5
    • /
    • pp.45-54
    • /
    • 2007
  • Time/frequency analysis has been extensively used in biomedical signal processing. By extracting some essential features from the electro-physiological signals, these methods are able to determine the clinical pathology mechanisms of some diseases. However, this method assumes that the signal should be stationary, which limits its application in non-stationary system. In this paper, we develop a new signal processing method using Hilbert-Huang Transform to perform analysis of the nonlinear and non-stationary ventricular fibrillation(VF). Hilbert-Huang Transform combines two major analytical theories: Empirical Mode Decomposition(EMD) and the Hilbert Transform. Hilbert-Huang Transform can be used to decompose natural data into independent Intrinsic Mode Functions using the theories of EMD. Furthermore, Hilbert-Huang Transform employs Hilbert Transform to determine instantaneous frequency and amplitude, and therefore can be used to accurately describe the local behavior of signals. This paper studied for Return Of Spontaneous Circulation(ROSC) and non-ROSC prediction performance by Support Vector Machine and three parameters(EMD-IF, EMD-FFT) extracted from ventricular fibrillation ECG waveform using Hilbert-Huang transform. On the average results of sensitivity and specificity were 87.35% and 76.88% respectively. Hilbert-Huang Transform shows that it enables us to predict the ROSC of VF more precisely.

Damage Detection of a Frame Structure Using Finite Element Model Updating (유한요소모델개선기법을 이용한 골조구조물의 손상탐지)

  • Yu, Eun-Jong;Kim, Seung-Nam;Lee, Hyun-Kook;Choi, Hang
    • Journal of the Computational Structural Engineering Institute of Korea
    • /
    • v.22 no.5
    • /
    • pp.445-452
    • /
    • 2009
  • In this paper, damage detection procedure using the finite element model updating was formulated and applied to a small-scale frame structure. FE model updating is the analytical method which finds the mathematical model that generates the measured dynamic properties similarly, and can be effectively used for the damage detection and SHM. For model updating, several kinds of dynamic properties, such as the natural frequencies, mode shapes, and frequency response functions, can be used as the inputs. In this paper, two kinds of model updating procedures using the natrual frequency and the frequency response function, and the natrual frequency and the mode shapes, respectively, were applied to identify the location and the severity of damage of the test structure, which is a four-story two bay steel structure. Results from the damage detection showed that more accurate identification results was obtained when the natrual frequency and the frequency response function were used than when the natrual frequency and the mode shapes were used.

Estimation of the Characteristics of Delayed Failure and Long-term Strength of Granite by Brazilian Disc Test (압열인장시험을 이용한 화강암의 지연파괴특성 및 장기안정성 평가)

  • Jung, Yong-Bok;Cheon, Dae-Sung;Park, Eui-Seob;Park, Chan;Lee, Yun-Su;Park, Chul-Whan;Choi, Byung-Hee
    • Tunnel and Underground Space
    • /
    • v.24 no.1
    • /
    • pp.67-80
    • /
    • 2014
  • Long-term stability and delayed failure of granite were evaluated through the laboratory test based on Wilkins method and Brazilian disc test (BDT) which yields tensile strength, mode I fracture toughness and subcritical crack growth parameters. Then, the long-term strength of granite was estimated by using analytical models and long-term stability of compressed air-energy storage (CAES) pilot cavern pressurized up to 5 ~ 6 MPa was evaluated using numerical code, FRACOD with the determined subcritical crack growth parameters. The results of test and analyses showed that the subcritical crack growth index, n was determined as 29.39 and the inner pressure of 5 ~ 6 MPa had an insignificant effect on the long-term stability of pilot cavern. It was also found that the measurement and analysis of acoustic emission events can describe the accumulation of damage due to subcritical crack growth quantitatively. That is, AE monitoring can provide the current status of rock under loading if we make an identical installation condition in the field with that of the laboratory test.

Analysis of Amineptine and its Metabolites in Human Urine by Gas Chromatography/Mass Spectrometry (Gas Chromatography/Mass Spectrometry를 이용한 뇨중 Amineptine과 그 대사체 분석방법에 관한 연구)

  • Lee, Jeong Ae;Kim, Younglim;Lho, Dong-Seok
    • Analytical Science and Technology
    • /
    • v.13 no.3
    • /
    • pp.385-393
    • /
    • 2000
  • A gas chromatography-mass spectrometric (GC/MS) procedure for the determination of amineptine (dihydro-10, 11-dibenzo[a, d] cycloheptenyl-5-amino-7-heptanoic acid) and its main metabolites in human urine was described. Amineptine has been known to be extensively metabolized by the ${\beta}$-oxidation of the heptanoic side chain with formation of pentanoic side chain metabolite ($C_5$-metabolite), and lactamizarion by internal dehydration of (${\beta}$-oxidized metabolite (${\delta}$-lactam). The detection of these compounds was based on acid hydrolysis, liquid-liquid extraction and trimethylsilylated derivatization of the carboxylic acid group. For the determination of amineptine and its metabolites in biological fluids, selected ions at the m/ 192, molecular ion and one of the characteristic ions were monitored by GC/MS. On the excretion study of amineptine in human urine, 70-90% of amineptine, ${\delta}$-lactam, and $C_5$-metabolite were found to be excreted within 4 hours and their excretion completed within 20 hours.

  • PDF

Comparison Solid Phase Microextraction with Purge & Trap on the GC/MS Analysis of Volatile Organic Compounds in Biota Samples (Solid Phase Microextraction 및 Purge & Trap을 이용한 생물시료 중 휘발성 유기화합물의 GC/MS 분석비교)

  • Ahn, Yun-Gyong;Seo, Jong-Bok;Hong, Jongki
    • Analytical Science and Technology
    • /
    • v.14 no.5
    • /
    • pp.392-399
    • /
    • 2001
  • The analysis of n-butylbenzene and 1,2-dibromo-3-chloropropane (DBCP) as volatile organic compounds in biota samples was performed by gas chromatography/mass spectrometry-selected ion monitoring mode. The target compounds, n-butylbenzene and DBCP, in biota samples were extracted by headspace solid phase microextraction (SPME) with $100{\mu}m$ polydimethyl siloxane (PDMS) fiber and purge & trap method. The extraction recoveries of these compounds obtained by SPME was 85.8% for n-butylbenzene and 92.4% for DBCP, respectively. Each value of method detection limit were $0.15{\mu}g/kg$ and $0.05{\mu}g/kg$, respectively. While in the case of purge & trap method, the extraction recovery was 115.2% for n-butylbenzene, 80.9% for DBCP and method detection limit were $0.04{\mu}g/kg$ and $0.70{\mu}g/kg$, respectively. The extraction yields and detection limits of these compounds obtained by purge & trap were equivalent to those by SPME.

  • PDF

A Review for Non-linear Models Describing Temperature-dependent Development of Insect Populations: Characteristics and Developmental Process of Models (비선형 곤충 온도발육모형의 특성과 발전과정에 대한 고찰)

  • Kim, Dong-Soon;Ahn, Jeong Joon;Lee, Joon-Ho
    • Korean journal of applied entomology
    • /
    • v.56 no.1
    • /
    • pp.1-18
    • /
    • 2017
  • Temperature-dependent development model is an essential component for forecasting models of insect pests as well as for insect population models. This study reviewed the nonlinear models which explain the relationship between temperature and development rate of insects. In the present study, the types of models were classified largely into empirical and biophysical model, and the groups were subdivided into subgroups according to the similarity of mathematical equations or the connection with original idea. Empirical models that apply analytical functions describing the suitable shape of development curve were subdivided into multiple subgroups as Stinner-based types, Logan-based types, performance models and Beta distribution types. Biophysical models based on enzyme kinetic reaction were grouped as monophyletic group leading to Eyring-model, SM-model, SS-mode, and SSI-model. Finally, we described the historical development and characteristics of non-linear development models and discussed the availability of models.

Flexural Behaviors of Reinforced Concrete Beams Strengthened with Carbon Fiber Sheets (탄소섬유시트로 보강된 철근콘크리트 보의 휨 거동)

  • Kim, Seong-Do
    • Journal of the Computational Structural Engineering Institute of Korea
    • /
    • v.23 no.2
    • /
    • pp.227-234
    • /
    • 2010
  • To investigate the flexural behavior of RC beams strengthened with carbon fiber sheets, 1 control beam and 8 strengthened beams(4 NU-beams without U-shaped band and 4 U-beams with U-shaped band) are tested. The variables of experiment are composed of the number of carbon fiber sheets and the existence of U-shaped band, etc. The experimental results showed that the strengthening system with U-shaped band controls the premature debonding and provides a more ductile failure mode than the strengthening system without U-shaped band. It can be found from the load-deflection curves that as the number of fiber sheets is increased, the maximum strength and the flexural rigidity is increased. The experimental results are compared with the analytical results of nonlinear flexural behaviors for strengthened RC beam. The proposed analytical method for strengthened beams is proved to be accurate by an experimental investigation of load-deflection curve, yield load, maximum load, and flexural rigidities in the pre- and post-yielding stages.

Characteristics Analysis of RPV and AFD for Anti-Islanding in Active Method (단독운전방지를 위한 능동 방식 중 AFD 및 RPV에 대한 특성해석)

  • Choe, Gyu-Ha;D, Bayasgalan;Lee, Young-Jin;Han, Dong-Ha;Jeong, Byong-Hwan;Kim, Hong-Sung
    • The Transactions of the Korean Institute of Power Electronics
    • /
    • v.14 no.2
    • /
    • pp.160-167
    • /
    • 2009
  • To detect islanding mode when the grid is being tripped is a major safety issue in the Utility Interactive Photo Voltaic (UIPV) system. In this paper, analytical design method is suggested for AFD & RPV method under IEEE 929-2000 recommended islanding test condition. We have discussed that there is a same point. we injected reactive component of the current by AFD & RPV methods, but the current reference generated is other waveform. Possible if amount of reactive components in this methods are same each method, there is happened same rates frequency variation. To verify the validity of the analytical comparison, this paper presents simulation and experimental results from single phase, 3[kW] inverter for the transformerless UIPV system.