• Analytical Science and Technology
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• v.20 no.2
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• pp.138-146
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• 2007

A simple and sensitive method for the determination of paroxetine in canine plasma was developed and validated by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry (LC-/MS/MS). Fluoxetine was used as an internal standard. Paroxetine and internal standard in plasma samples were extracted using TBME (tert-butyl methyl ether). A centrifuged upper layer was then evaporated and reconstituted with mobile phase of 50% acetonitrile adjusted to pH 3 by formic acid. The reconstituted samples were injected into a Capcell Pak UG120 ($2.0{\times}150mm$, $5{\mu}m$) column. Using MS/MS with SRM (selective reaction monitoring) mode, the transitions (precursor to product) monitored were m/z $330{\rightarrow}192$ for paroxetine, and m/z $310{\rightarrow}148$ for internal standard. Linear detection responses were obtained for paroxetine concentration range of 0.02~5 ng/mL. A correlation coefficient of linear regression ($R^2$) was 0.9993. Detection of paroxetine in canine plasma was accurate and precise, with limit of quantification at 0.02 ng/mL. The method has been successfully applied to pharmacokinetic study of paroxetine in healthy beagle dogs.

• Journal of Food Hygiene and Safety
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• v.8 no.1
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• pp.9-15
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• 1993

In an attempt to quantitate and qualitate residual antibiotics and antibacterial agents in meat simultaneously, we studied a gas chromatography-mass spectrometry(GC/M8) analysis. For a simultaneous analysis of penicillin G, chloramphenicol and thiamphenicol in meat, a simple and rapid clean-up procedure including extraction with 0.01 M EDTA-2Na Mcilvaine buffer (pH 4.0), defatting with n-hexane, and elution with 0.01M-methanolic oxalic acid from Bond Elute $C_{18}$ cartridge, and quantitation by selected ion monitoring (SIM) mode after derivatization was performed. The recoveries (%) of penicillin G, chloramphenicol and thiamphenicol (CV, %) at 1 ppm fortification level were 63.5 (7.6), 76.3 (8.1) and 84.7 (2.0), and the detection limits of those were 0.6, 0.085 and $0.084\;\mu\textrm{g}$ beef, respectively. This method using 81M mode allows excellent detection and quantitation of residual antibiotics and antibacterial agents in meat. Moreover, confirmation by a full scan electron impact mass spectrum is possible if residual level in the sample in above 1 ppm.

• Journal of Food Hygiene and Safety
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• v.32 no.3
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• pp.193-198
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• 2017

Scutellaria baicalensis, Eleutherococcus senticosus, and Angelica sinensis have been used as raw materials for health functional foods. This study was conducted to develop a novel method to analyze levels of baicalin (Scutellaria baicalensis), eleutheroside E (Eleutherococcus senticosus), and ligustilide (Angelica sinensis) simultaneously in health functional foods. The methanol extracted samples were analyzed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode and the negative ion mode using multiple reaction monitoring. Standard calibration curves confirmed linearity with the correlation coefficient ($r^2$) of > 0.99 at $100-2000{\mu}g/mL$ concentration range. The limits of detection (LODs) and limits of quantitation (LOQs) were in the range of $13.0{\sim}35.2{\mu}g/L$ and $39.3{\sim}106.7{\mu}g/L$, respectively. The recovery results ranged between 91.4~109.9% at 3 different concentration levels with relative standard deviations (RSDs) less than 5%. The proposed analytical method was characterized with high accuracy and acceptable precision. The new method would be an effective tool to analyze baicalin, eleutheroside E, and ligustilide simultaneously in raw materials of health functional foods.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.2 no.2
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• pp.97-104
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• 2004

Neutron induced prompt gamma-ray spectroscopy(NIPS) system measures the prompt gamma-ray emitting by the interaction of a neutron with various materials. This system will be of great benefit to scientists worldwide, since it provides the non-destructive measurement of many element in either solid or liquid wastes. In this study, the full-energy-peak (FEP) efficiency calibration for a HPGe detector was constructed in the ${\gamma}$-ray energy range from 80 keV to 8 MeV, using $^{l33}$Ba and >TEX>$^{152}Eu$ RI sources and $ ^{35}Cl(n, ${\gamma}$)^{36}Cl$ thermal neutron captured reaction. The FEP efficiency curve for the higher energies using the $^{35}Cl(n, ${\gamma}$)^{36}Cl$ reaction was normalized with the curve obtained from the RI sources, since the accurate activity of its prompt ${\gamma}$-ray is unknown. The average thermal neutron flux was theoretically calculated using the FEP efficiency curve for the KCl standard solutions. The NIPS system equipped with a ${\gamma}$-${\gamma}$ coincidence setup with two n-type coaxial HPGe detectors was considered in order to reduce the interfering ${\gamma}$-ray background. The FEP efficiency curve for the ${\gamma}$-${\gamma}$ coincidence system was also obtained for full energy range. The performance of the normal and coincidence NIPS system was tested by comparing signal-to-noise ratio in each mode using the reference sample.e.

• Analytical Science and Technology
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• v.26 no.4
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• pp.221-227
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• 2013

A sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the investigation of the ginsenoside Rg1 in human plasma. After addition of internal standard (digoxin), plasma was diluted with acetone and methanol (80:20), the supernatant was concentrated and analyzed by LC-MS/MS. The optimal chromatographic separation was achieved on an Agilent Eclipse XDB-C18 column ($4.6{\times}150mm$, $5{\mu}m$) with a mobile phase of 0.1% formic acid in water and 0.1% formic acid in methanol at a flow rate of 0.9 mL/min gradient mode. The standard calibration curve for ginsenoside Rg1 was linear ($r^2=0.9995$) over the concentration range 1~500 ng/mL in human plasma. The intra- and inter-day precision over the concentration range of ginsenoside Rg1 was lower than 7.53% (correlation of variance, CV), and accuracy exceeded 98.28%. This LC-MS/MS assay of ginsenoside Rg1 in human plasma is applicable for quantifying in the pharmacokinetic study.

• Korean Journal of Applied Biomechanics
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• v.18 no.4
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• pp.109-114
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• 2008

The purpose of this study was to estimate the energy expenditure simply and practically during physical activities. The physical activity is quantified by the integration of the accelerometer signals obtained from the triaxial accelerometer attached at the waist level of the human body. To find a relationship between energy expenditure and accelerometer data, 6 male and 5 female subjects walked and ran on the treadmill with speeds of 1.5, 3.0, 4.5, 6.0, 6.5, 7.0, and 8.5 km/hr. Each subject performed walking at the speed lower than 6.0 km/hr and running at the speed higher than 6.5 km/hr. Actual energy expenditure was determined by a continuous direct gas analyzer. Two predictive equations of walking and running mode for energy expenditure which includes gender, body mass index(BMI) and data from accelerometer were developed using multiple regression analysis. The correlation coefficients and coefficients of determination between the estimated and measured energy expenditure were R=0.936, R2=0.876 and R=0.881, R2=0.776 in walking and running mode, respectively. For further study, experiments on a larger scale of test subjects are essential for acquiring more reliable results.

• Analytical Science and Technology
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• v.31 no.1
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• pp.23-30
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• 2018

Twenty-two allergy-induced aromatics in children were analyzed using a gas chromatography flame ionization detector (GC-FID) and gas chromatography mass spectrometer (GC-MSD). Analytes were extracted using an automatic Soxhlet extractor and centrifuged for 10 min in a fast freezing centrifuge, and the supernatant was transferred into a 2 mL vial and injected in split mode. Under the established conditions, the calibration curve showed linearity with a correlation coefficient of 0.996 or more. A wide range of sensitivity of 6.7 to 1,859,839 depending on the device characteristics and detector used was shown. The detection limit of the device was 0.0032 to $0.0335{\mu}g/mL$, and the maximum detection limit was less than $0.1{\mu}g/mL$. The detection limit of the method ranged from 0.0033 to $0.1161{\mu}g/mL$. In addition, the limit of quantification ranged from 0.0100 to $0.5422{\mu}g/mL$, with a level of precision ranging from 0.21 % to 4.89 % and a degree of accuracy ranging from 89 % to 111 %. The analytical method developed in this study was applied to commercial products.

• Analytical Science and Technology
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• v.31 no.1
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• pp.39-46
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• 2018

Carbaryl and seven organophosphorous pesticides were analyzed simultaneously using on-line solid phase extraction (on-line SPE) coupled with liquid chromatography tandem mass spectrometry (LC/MS/MS). The target pesticides are Carbaryl, Methyl demeton, Fenitrothion, Malathion, Parathion, Phenthoate, Diazinon, and EPN. This method includes the direct injection of $500{\mu}L$ in the water sample, a 15 min separation period using a rapid resolution liquid chromatography system with on-line SPE, and detection through electrospray ionization (ESI) positive mode. The percentage of recovery of all pesticides ranged from 85.3 % to 100 %. This method showed an accuracy of ${\geq}90.0%$, possessing limits of detection and quantification within 0.05 to $0.28{\mu}g/L$ and 0.16 to $0.89{\mu}g/L$, respectively. The correlation coefficients (r) for the calibration curves within a range of 0.5 to $8.0{\mu}g/L$ were higher than 0.99. The evaluation results showed the efficacy of the method for all contents, and no pesticides were detected in the water quality sample.

• Analytical Science and Technology
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• v.18 no.2
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• pp.163-167
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• 2005

In this study, a novel analytical method has been developed for the rapid determination of L-carnitine in human plasma using electrospray ionization tandem mass spectrometry. Free carnitine (FC) was analyzed after extraction with 80% methanol and total carnitine (TC) was analyzed after hydrolysis and extraction. Acyl carnitine (AC) was subtracted FC from TC. Analytical methods used multiple reaction monitoring (MRM) scan modes. A correlation coefficient of linear regression ($r^2$) was 0.9995, recovery was 97%, reproducibility was less than 10%, and limit of detection (LOD) was $0.0016{\mu}mol/L$. This method reduced sample preparation time and showed high resolution and good reproducibility compared to that with liquid chromatographic methods. Normal control showed AC was lower than FC. Clinical management of patients with inborn error of metabolism showed FC was lower than AC. Thus, carnitine fraction level was very important to monitoring patients with metabolic disorder.

• Proceedings of the Korean Society for Technology of Plasticity Conference
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• 2009.10a
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• pp.223-226
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• 2009

The plastics are widely utilized in the inside of vehicles. The dynamic tensile characteristics of auto-body plastics are important in a prediction of deformation mode of the plastic component which undergoes the high speed deformation during car crash. This paper is concerned with the dynamic tensile characteristics of the auto-body plastics at intermediate strain rates. Quasi-static tensile tests were carried out at the strain rate ranged from 0.001/sec to 0.01/sec using the static tensile machine(Instron 5583). Dynamic tensile tests were carried out at the strain rate ranged from 0.1/sec to 100/sec using the high speed material testing machine developed. Conventional extensometry method is no longer available for plastics, since the deformation of plastic is accompanied with localized deformation. In this paper, quasi-static and dynamic tensile tests were performed using ASTM IV standard specimens with grids and images from a high speed camera were analyzed for strain measurement. True stress-strain relations and the actual strain rates at each deformation step were obtained by processing load data and deformation images, assuming the plastics to deform uniformly in each grid.