• Korean Journal of Pharmacognosy
• /
• v.44 no.4
• /
• pp.350-361
• /
• 2013

Asarum sieboldii has been used for treatment of fever, pain, common cold, and chronic sinusitis in Korea. In this study, we performed quantification analysis of seven major constituents including aristolochic acid I, aristolochic acid II, ${\alpha}$-asarone, ${\beta}$-asarone, elemicin, methyl eugenol, and safrole in the 70% ethanol extract of Asarum sieboldii and its solvent fractions, n-hexane, ethylacetate, n-butanol, and water ones using a ultra-performance liquid chromatography-electrospray ionization-mass spectrometer(UPLC-ESI-MS) and gas chromatography-mass spectrometer(GC-MS). Regression equations of seven components were acquired with $r^2$ values >0.99. The values of limit of detection(LOD) and quantification(LOQ) were 0.1-3.9 ng/mL and 0.3-11.7 mg/mL, respectively. The amount of the seven compounds in Asarum sieboldii were not detected -143.66 mg/g. The established LC-MS/MS and GC-MS methods will be helpful to improve quality control of Asarum sieboldii.

• Analytical Science and Technology
• /
• v.25 no.1
• /
• pp.83-90
• /
• 2012

The objective of the study was to estimate the measurement uncertainty associated with determination of creatinine (Cr) in urine samples by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Centrifuged urine samples (10 ${\mu}L$) were diluted with 390 ${\mu}L$ of distilled water. To 20 ${\mu}L$ aliquots of diluted urine samples, 30 ${\mu}L$ of internal standard solution (Cr-$d_3$, 5 ${\mu}g/mL$) and 10 ${\mu}L$ of acetonitrile were added and filtered. The samples (1 ${\mu}L$) were introduced into LC-MS/MS with no further pretreatment. Cr was separated on a multi-mode ODS column (Scherzo SM-C18, 75 ${\times}$ 2.0 mm I.D., 3 ${\mu}m$) and quantified by LC-MS/MS operating in MRM mode (Cr, m/z 114.0${\rightarrow}$ 86.0; Cr-$d_3$, m/z 117.0${\rightarrow}$ 89.1). The four factors that contribute uncertainty to the final result were extracted and evaluated. The principal factors of contribution to combined standard uncertainty were sample dilution, calibration curve and repeatability, while the preparation of standard solution was only a minor factor. Relative extended uncertainty of the measured concentration was 14.2% in a real urine sample.

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

• Analytical Science and Technology
• /
• v.23 no.4
• /
• pp.414-422
• /
• 2010

In forensic examinations of question document, analysis about inks components and the dating of ink entries is often of considerable importance and forensic examination of inks is principally concerned with the classification and comparison of chemically complex mixtures. The authenticity about inks analysis of a questioned document may be examined through the analysis of inks used to TLC, HPLC/MS, GC/MS, LDI/MS. We collected 56 difference types of black ballpoint pen inks manufactured from 5 country groups. We identified major 6 species volatile organic components (VOCs), ethylbenzene ($0.089-0.244\;{\mu}g$/mL), o-xylene ($0.072-0.331\;{\mu}g$/mL), m,p-xylene ($0.062-0.318\;{\mu}g$/mL), benzene ($0.003-0.173\;{\mu}g$/mL), 1,1-dichloroethylene ($0.003-0.295\;{\mu}g$/mL), toluene ($0.007-0.484\;{\mu}g$/mL) using HS-SPME GC/MS. The results of this study indicated that determined VOCs of black ballpoint pen inks could make a discriminating tool of inks analysis for forensic question document and can supply methodology for classification and identification of between ballpoints pen inks.

• Journal of the Korean Society of Radiology
• /
• v.5 no.6
• /
• pp.401-407
• /
• 2011

The purpose of this study is to know the differences of MR spectra, obtained from normal volunteers by variable TE value, through the quantitative analysis of brain metabolites by peak integral and SNR between 1.5T and 3.0T, together with PRESS and STEAM pulse sequence. Single-voxel MR proton spectra of the human brain obtained from normal volunteers at both 3.0T MR system (Magnetom Trio, SIEMENS, Germany) and 1.5T MR system (Signa Twinspeed, GE, USA) using the STEAM and PRESS pulse sequence. 10 healthy volunteers (3.0T:3 males, 2 females; 1.5T : 3 males, 2 females) with the range from 22 to 30 years old (mean 26 years) participated in our study. They had no personal or familial history of neurological diseases and had a normal neurological examination. Data acquisition parameters were closely matched between the two field strengths. Spectra were recorded in the white matter of the occipital lobe. Spectra were compared in terms of resolution and signal-to-noise ratio(SNR), and echo time(TE) were estimated at both field strengths. Imaging parameters was used for acquisition of the proton spectrum were as follow : TR 2000msec, TE 30ms, 40ms, 50ms, 60ms, 90ms, 144ms, 288ms, NA=96, VOI=$20{\times}20{\times}20mm3$. As the echo times were increased, the spectra obtained from 3.0T and 1.5T show decreased peak integral and SNR at both pulse sequence. PRESS pulse sequence shows higher SNR and signal intensity than those of STEAM. Especially, Spectra in normal volunteers at 3.0T demonstrated significantly improved overall SNR and spectral resolution compared to 1.5T(Fig1). The spectra acquired at short echo time, 3T MR system shows a twice improvement in SNR compared to 1.5T MR system(Table. 1). But, there was no significant difference between 3.0Tand 1.5T at long TE It is concluded that PRESS and short TE is useful for quantification of the brain metabolites at 3.0T MRS, our standardized protocol for quantification of the brain metabolites at 3.0T MRS is useful to evaluate the brain diseases by monitoring the systematic changes of biochemical metabolites concentration in vivo.

• Korean Journal of Pharmacognosy
• /
• v.49 no.3
• /
• pp.270-277
• /
• 2018

Pyungwi-san has been used to treat the digestive system diseases, physconia, nausea, anorexia, and dyspepsia in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was optimized for simultaneous determination of the 14 marker components, spinosin, liquiritirn apioside, liquiritin, narirutin, 6'''-feruloylspinosin, hesperidin, liquiritigenin, glycyrrhizin, 6-gingerol, atractylenolide III, honokiol, atractylenolide II, magnolol, and atractylenolide I in Pyungwi-san extract. All analytes were separated on a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) with maintained at $45^{\circ}C$. The mobile phase consisted of 0.1% (v/v) aqueous formic acid and acetonitrile. The MS conditions were as follows: capillary voltage 3.3 kV, extractor voltage 3.0 V, RF lens voltage 0.3 V, source temperature $120^{\circ}C$, desolvation temperature $300^{\circ}C$, desolvation gas 600 L/h, cone gas 50 L/h and collision gas 0.14 mL/min. The coefficient of determination of 14 analytes was 0.9989-1.0000. The limits of detection and quantification values of the all analytes were 0.04-2.56 and 0.13-7.69 ng/mL, respectively. As a result of the analysis using the established LC-ESI-MS/MS method, the 5 components, spinosin, 6'''-feruloylspinosin, atractylenolide III, II, and I derived from Zizyphi Fructus and Atractylodis Rhizoma, were not detected in this extract. On the other hand, the 9 components except for the 5 components were 4.15-498.87 mg/kg in lyophilized Pyungwi-san extract. Among these components, glycyrrhizin, marker compound of Glycyrrhizae Radix et Rhizoma, was detected the most amount as a 498.87 mg/kg.

• Korean Journal of Pharmacognosy
• /
• v.48 no.4
• /
• pp.320-328
• /
• 2017

Yongdamsagan-tang has been used to treat the urinary disorders, acute- and chronic-urethritis, and cystitis in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was established for simultaneous analysis of the 20 bioactive marker compounds, geniposidic acid, chlorogenic acid, geniposide, liquiritin apioside, acteoside, calceolarioside B, liquiritin, nodakenin, baicalin, liquiritigenin, wogonoside, baicalein, glycyrrhizin, wogonin, glycyrrhizin, wogonin, saikosaponin A, decursin, decursinol angelate, alisol B, alisol B acetate, and pachymic acid in traditional herbal formula, Yongdamsagan-tang. Chromatographic separations of all marker compounds were conducted using a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) at $45^{\circ}C$ using a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. The MS analysis was performed using a Waters ACQUITY TQD LC-MS/MS coupled with an electrospray ionization source in the positive and negative modes. The flow rate was 0.3 mL/min and injection volume was $2.0{\mu}L$. The correlation coefficient of 20 marker compounds in the test ranges was 0.9943-1.0000. The limits of detection and quantification values of the all marker components were 0.11-6.66 and 0.34-19.99 ng/mL, respectively. As a result of the analysis using the optimized LC-ESI-MS/MS method, three compounds, geniposidic acid (from Plantaginis Semen), alisol B (from Alismatis Rhizoma), and pachymic acid (from Poria Sclerotium), were not detected in this sample. While the amounts of the 17 compounds except for the geniposidic acid, alisol B, and pachymic acid were $0.04-548.13{\mu}g/g$ in Yongdamsagan-tang sample. Among these compounds, baicalin, bioactive marker compound of Scutellariae Radix, was detected at the highest amount as a $548.13{\mu}g/g$.

• KOREAN JOURNAL OF CROP SCIENCE
• /
• v.29 no.1
• /
• pp.102-107
• /
• 1984

This study was undertaken to know the possibility of in vitro propagation of Stevia through axillary bud culture and the results indicated that: (1) Addition of NAA (0.01-0.05 mg/l) alone on Murashige-Skoog basal medium promoted shoot differentiation and growth rate. And also additional of kinetin of 0.5-1.0 mg/1 alone showed the same trend as that of NAA: (2) Addition of both NAA (0.01-0.05 mg/l) and kinetin (0.5-1.0mg/l) to MS medium promoted better shoot formation. (3) Shoot differentiation and growth were better on the full salt strength of MS medium (1X MS) than that of half strength ( $\frac{1}{2}$MS), while their effects were reversed for root differentiation

• Korean Journal of Plant Tissue Culture
• /
• v.22 no.6
• /
• pp.307-310
• /
• 1995

Cotyledon and epicotyl explants of P. aridum and P. zonale formed calli when cultured on MS medium supplemented with 2 mg/L NAA and 0.2 mg/L BA. Calli were subcultured on the same medium Upon transfer to MS medium with 0.1 to 0.5mg/L NAA and 0.25 to 2mg/L BA for P. aridum 0.1 to 0.5mg/L NAA and 1 to 2mg/L BA for P. zonale subcultured calli gave rise to the greatest number of shoots (0.78 shoot for P. aridum and 0.65 shoot per explant for P. zonale, respectively).Most shoots produced roots when cultured on 1/2MS basal medium. The regenerates were transferred to potting soil and grown to materity in a greenhouse.

• Korean Journal of Fisheries and Aquatic Sciences
• /
• v.54 no.4
• /
• pp.404-410
• /
• 2021

Although, mouse bioassay for the monitoring of azaspiracids (AZAs) toxins in shellfish has been used previously, the reported method has low sensitivity and it is time-consuming. Recently, there is an interest in the quantitative analysis of AZAs using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The purpose of this study is to verify the simultaneous analysis of AZAs in shellfish and tunicate in Korea using LC-MS/MS. To validate the method, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy, and repeatability were determined. All standard compounds were analyzed within 7 min. The correlation coefficients (R²) of the standard solution was higher than 0.9995 (within the range of 0.8-10.0 ㎍/L). The LODs and LOQs of AZAs in shellfish were 0.08-0.16 ㎍/kg and 0.23-0.50 ㎍/kg, respectively. The accuracy and precision of the method for determining AZAs in shellfish were 87.1-93.0% and 1.23-4.91%, respectively. Consequently, the verified LC-MS/MS method is suitable to analyze AZAs in shellfish and tunicates in Korea.