• Journal of the Korean Society of Tobacco Science
• /
• v.30 no.2
• /
• pp.117-124
• /
• 2008

A solid phase microextraction (SPME) method in combination with gas chromatography/mass spectrometric techniques was used for the extraction and quantification of 12 selected agrochemical residues in tobacco. The parameters such as the type of SPME fiber, adsorption/desorption time and the extraction temperature affecting the precision and accuracy of the SPME method were investigated and optimized. Among three types of fibers investigated, polyacrylate (PA), polydimethylsiloxane (PDMS) and polydimethylsiloxane-divinylbenzene (PDMS-DVB), PDMS fiber was selected for the extractions of the agrochemicals. The SPME device was automated and on-line coupled to a gas chromatograph with a mass spectrometer. Mass spectrometry (MS) was used and two different instruments, a quadrupole MS and triple quadrupole MS-MS mode, were compared. The performances of the two GC-MS instruments were comparable in terms of linearity (in the range of 0.01$\sim$0.5 $\mu$g/mL) and sensitivity (limits of detection were in the low ng/mL range). The triple quadrupole MS-MS instrument gave better precision than that of quadrupole MS system, but generally the relative standard deviations for replicates were acceptable for both instruments (< 15%). The LODs was fully satisfied the requirements of the CORESTA GRL. Recoveries of 12 selected agrochemicals in tobacco yielded more than 80% and reproducibility was found to be better than 10% RSD so that SPME procedure could be applied to the quantitative analysis of agrochemical residues in tobacco.

• Journal of Ginseng Research
• /
• v.41 no.1
• /
• pp.10-22
• /
• 2017

Background: Asian ginseng and American ginseng are functional foods that share a close genetic relationship and are well-known worldwide. This article aims to investigate the correlation between morphological characteristics and the inherent quality of Asian and American ginsengs. Methods: In this study, an ultra-HPLC-quadrupole/time-of-flight MS (UHPLC-Q/TOF-MS) method was established for the quantitative analysis of 45 ginseng samples. The method developed for determination was precise and accurate. Results: The results showed that Asian ginseng samples with the same growing time (with the same or similar number of stem scars) that had a thinner main root, a longer rhizome and more branch roots contained greater amounts of ginsenosides. For American ginseng, two tendencies were observed in the relationship between the diameter of the main root and contents of ginsenosides. One tendency was that samples with thinner main roots tended to contain higher levels of ginsenosides, which was observed in the samples sold under the commercial name pao-shen. Another tendency was that samples with thicker main roots contained higher contents of ginsenosides, which was observed in the samples sold under the commercial name pao-mian, as well as in samples of American ginseng cultivated in Jilin, China. Conclusion: An approach using ultra-HPLC-quadrupole/time-of-flight MS was successfully established to link morphology and active components for evaluating the quality of Asian and American ginsengs. Clear correlation between visible morphological features and quality of Asian and American ginsengs was found. People can see the difference; this means consumers and vendors can evaluate ginseng by themselves.

• Mass Spectrometry Letters
• /
• v.6 no.4
• /
• pp.105-111
• /
• 2015

Sixteen compounds of Neobalanocarpus heimii were successfully identified directly from their plant extract using a triple quadrupole LC-MS/MS system. In order to fulfil the objectives of this work, a series of stilbene oligomers of various degrees of condensation were isolated and their structure are characterized. Out of these, four are resveratrol dimers, three trimers, and nine tetramers. The isolation process was done on a fully automated semi-preparative HPLC system. Their structures were elucidated on the basis of 1D- and 2D-NMR as well as MS data. The mass fragmentation patterns of the compounds were recorded and a retrievable in-house library was built to keep the data. In order to demonstrate the potential of this approach, the polyphenolic crude extract was analysed with the LC-MS/MS system and the MS/MS spectra extracted for each chromatographic peak of interest. The fragmentation patterns were compared with those of anticipated pure compounds that were previously recorded. All compounds were successfully identified. It is therefore believed that the LC-MS/MS potential for dereplication of structurally similar compounds in a crude mixture was thus firmly established.

• Journal of Ginseng Research
• /
• v.40 no.4
• /
• pp.382-394
• /
• 2016

Background: Ginsenosides are the characteristic and principal components which manifest a variety of the biological and pharmacological activities of the roots and rhizomes of Panax ginseng (GRR). This study was carried out to qualitatively and quantitatively determine the ginsenosides in the cultivated and forest GRR. Methods: A rapid and sensitive ultra-high-performance liquid chromatography coupled with diode-array detector and quadrupole/time of flight tandem mass spectrometry (UPLC-DAD-QTOF-MS/MS) was applied to the qualitative analysis of ginsenosides and a 4000 QTRAP triple quadrupole tandem mass spectrometer (HPLC-ESI-MS) was applied to quantitative analysis of 19 ginsenosides. Results: In the qualitative analysis, all ingredients were separated in 10 min. A total of 131 ginsenosides were detected in cultivated and forest GRR. The method for the quantitative determination was validated for linearity, precision, and limits of detection and quantification. 19 representative ginsenosides were quantitated. The total content of all 19 ginsenosides in the forest GRR were much higher than those in the cultivated GRR, and were increased with the growing ages. Conclusion: This newly developed analysis method could be applied to the quality assessment of GRR as well as the distinction between cultivated and forest GRR.

• Journal of the Korean Society of Tobacco Science
• /
• v.29 no.2
• /
• pp.132-139
• /
• 2007

This study was performed to apply the more rapid and accurate sample preparation, and the high selectivity and sensitivity of the analyte detection by gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). QuEChERS (quick, easy, cheap, effective, rugged and safe) method was validated for 49 agrochemicals in the CORESTA Agrochemical Advisory Committee guide and amenable to GC-MS/MS determination. In QuEChERS method, the effects of sorbents (PSA, $C_{18}$ and GCB) and matrix of the analytes in tobacco types (flue-cured, burley and oriental) were investigated. MS/MS acquisition provided high specificity and selectivity for agrochemicals and low limit of quantification. QuEChERS by using PSA alone and the matrix-matched standards gave good recoveries and RSD values in three types of tobaccos. QuEChERS method was no needed to be complex clean-up procedure and would be used as the fast and easy method for agrochemical residue analysis in tobacco.

• Mass Spectrometry Letters
• /
• v.1 no.1
• /
• pp.21-24
• /
• 2010

The development of clinical biomarkers involves discovery, verification, and validation. Recently, multiple reaction monitoring (MRM) coupled with stable isotope dilution mass spectrometry (IDMS) has shown considerable promise for the direct quantification of proteins in clinical samples. In particular, multiple biomarkers have been tracked in a single experiment using MRM-based MS approaches combined with liquid chromatography. We report here a highly reproducible, quantitative, and dynamic MRM system for validating multi-biomarker proteins using Nanoflow HPLC-Microfluidics Chip/Triple-Quadrupole MS. In this system, transitions were acquired only during the retention window of each eluting peptide. Transitions with the highest MRM-MS intensities for the five target peptides from colon cancer biomarker candidates were automatically selected using Optimizer software. Relative to the corresponding non-dynamic system, the dynamic MRM provided significantly improved coefficients of variation in experiments with large numbers of transitions. Linear responses were obtained with concentrations ranging from fmol to pmol for five target peptides.

• Mass Spectrometry Letters
• /
• v.12 no.4
• /
• pp.172-178
• /
• 2021

HYIpro-3-1 is an adjuvant for preventing or treating inflammatory growth diseases. In this study, we identified the metabolic pathway of HYIpro-3-1 in human liver microsomes (HLMs) by quadrupole-orbitrap high-resolution mass spectrometry (HR-MS) and characterized the major human cytochrome P450 (CYP). Ten metabolites were identified, including one O-demethylation (M1), two O-demethylation and monohydroxylation (M2 and M3), and seven monohydroxylation metabolites (M4-M10). Based on the HR-MS² spectra, the metabolites are divided into two groups of monohydroxylated metabolites according to the hydroxylation position. We verified that HYIpro-3-1 is metabolized by CYP in HLMs, CYP2B6 is mainly involved in O-demethylation, and various CYPs are involved in the monohydroxylation of HYIpro-3-1.

• Mass Spectrometry Letters
• /
• v.10 no.2
• /
• pp.61-65
• /
• 2019

Korean ginseng (Panax ginseng Meyer) is a traditional herb used across the world to treat various diseases. Although, red ginseng is this herb's most famous product and has demonstrated diverse pharmacological activities, white ginseng (WG) is another ginseng product that is made fresh and individually regulated in Eastern Asia. Red and white ginseng show different characteristics due to distinct processing steps despite originating from the same plant, and the drug interactions induced by WG have not been well documented. Selegiline is a selective monoamine oxidase (MAO) inhibitor used as an antidyskinetic and antiparkinsonian agent. Here we developed a quantification method for selegiline in mouse plasma using a C8 stationary phase in triple quadrupole-mass spectrometry (LC-MS/MS) with multiple reaction monitoring (MRM). The validated LC-MS/MS method was successfully applied to determine the potential interaction with WG extract (0.1 g/kg/day) pre-administered for 4 weeks. The $AUC_{0-240min}$ of selegiline was altered due to a decrease in the absorption of selegiline with repeated administration of WG extract.

• Bulletin of the Korean Chemical Society
• /
• v.25 no.4
• /
• pp.447-451
• /
• 2004

Low and high resolution inductively coupled plasma mass spectrometry (ICP-MS) coupled with ion chromatography (IC) has been investigated for speciation of Cr(III) and Cr(VI). In particular, the interference of ArC^+formed by the carbon in a sample on the simultaneous determination of Cr(III) and Cr(VI) has been studied. In chemical speciation, this study shows that quadrupole type ICP-MS with low resolution has a limitation of simultaneous determination fo chromium species if the sample contains the carbon elements. The interference problems can be solved by high resolution ICP-MS.

• Food Science of Animal Resources
• /
• v.43 no.6
• /
• pp.975-988
• /
• 2023

The fatty acid composition and small molecular metabolites in breast and leg meat of Yanjin blackbone chickens (YBC) and Piao chickens (PC) were detected by gas chromatography-mass spectrometry and liquid chromatography-quadrupole static field orbital trap mass spectrometry. Thirty-two fatty acids were detected, and the total fatty acid content of PC was significantly higher than that of YBC (p<0.05). Oleic acid, linoleic acid, palmitic acid, stearic acid, and arachidonic acid were the main fatty acids in the two chicken varieties, and the composition of fatty acids in the two varieties were mainly unsaturated fatty acids, being more than 61.10% of the total fatty acids. Meanwhile, 12 and 16 compounds were screened out from chicken legs and chicken breasts of YBC and PC, respectively, which had important contributions to the differences between groups.