• Journal of Life Science
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• v.19 no.12
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• pp.1698-1704
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• 2009

Gemcitabine is an anticancer drug used to treat a variety of solid tumors. The drug is rapidly inactivated by cytidine deaminase in plasma and its hydrophilicity restricts the extent of quantification that is possible using reversed-phase liquid chromatography. In this paper, we report a rapid and precise method to analyze velocity and peak efficiency using ultra-performance liquid chromatography (UPLC) with a reversed-phase column. The retention periods of gemcitabine and 2'-deoxycytidine at 283 nm were 3.2 and 2.1 min, respectively. The assay provided highly linear results in the range of $0.1{\sim}20{\mu}g/ml$ ($r^2$ > 0.999). The coefficients of variation of the intra-day and inter-day assays were less than 10.0%. We observed that the estimated average concentrations of the intra-day and inter-day assays ranged from 97.3 to 113.5% to verify the accuracy. These results suggest that this new reversed-phase UPLC method is a rapid and reliable way of determining gemcitabine levels.

• Analytical Science and Technology
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• v.30 no.4
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• pp.194-204
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• 2017

Direct injection (DI) and solid phase extraction (SPE) methods for the simultaneous determination of pendimethalin (PDM) and dinoseb (DNS) in environmental water have been optimized using the ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method. The limits of quantification (LOQs) of PDM and DNS were $0.01{\mu}g/L$ using the DI method and $0.0001-0.0002{\mu}g/L$ using the SPE method. The precision by SPE UPLC-MS/MS was less than 11 % for intra-day and inter-day analyses. When the proposed SPE method was used to analyze two analytes in environmental water, PDM was detected in a concentration range of $0.0002-0.011{\mu}g/L$ in 31 samples of the 114 surface water samples, and DNS was detected in a concentration range of $0.0005-0.045{\mu}g/L$ in 17 samples of the 114 surface water samples analyzed. When the DI method was used to analyze target compounds in the same samples, the detected concentrations of the two analytes were within 21% in samples with concentrations above $0.01{\mu}g/L$. The DI UPLC-MS/MS method can thus be used for the routine monitoring of PDM and DNS in environmental water, and the SPE LC-MS/MS method can be used for the determination of the ultra-trace PDM and DNS residues in environmental water.

• Natural Product Sciences
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• v.20 no.3
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• pp.182-190
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• 2014

An ultra-performance liquid chromatography (UPLC) coupled with electrospray ionization (ESI) tandem mass spectrometry (MS) method was established for quantitative analysis of twelve components, allantoin (1), morroniside (2), 5-hydroxymethyl-2-furfural (5-HMF) (3), loganin (4), coumarin (5), cinnamic acid (6), mesaconitine (7), cinnamaldehyde (8), hypaconitine (9), aconitine (10), alisol B (11), and alisol B acetate (12) in a Palmijihwang-hwan decoction. The twelve constituents were separated on a UPLC BEH C18 column ($2.1{\times}100mm$, $1.7{\mu}m$) at a column temperature of $40^{\circ}C$ by gradient elution with 0.1% (v/v) formic acid in water and acetonitrile as the mobile phase. The flow rate was 0.3 mL/min and the injection volume was $2.0{\mu}L$. Calibration curves of all compounds were acquired with values of the correlation coefficient ${\geq}0.99$ within the test ranges. The limits of detection and quantification for all analytes were 0.01 - 4.53 ng/mL and 0.03 - 13.60 ng/mL, respectively. The concentrations of the compounds 1 - 9 and 12 were 72.83, 4389.00, 4859.00, 3155.17, 223.67, 33.50, 1.97, 518.00, 2.25, and $25.00{\mu}g/g$, respectively. However, compounds 10 and 11 were not detected.

• Journal of the Korean Wood Science and Technology
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• v.44 no.3
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• pp.337-349
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• 2016

In this study, an analytical method to evaluate the quality of isoflavonoid compounds purified and isolated from the fruits of Cudrania tricuspidata was developed and validated using Ultra Performance Liquid Chromatography (UPLC). The fruits of C. tricuspidata were extracted with methanol and further fractioned with n-hexane, ethyl acetate and water. The resulting ethyl acetate extract separated into four isoflavonoid compounds by a combination of silica gel and sephadex LH-20 column chromatography. The structures of the compounds were elucidated as alpinumisoflavone, 6,8-diprenyl genistein, 6,8-diprenyl orobol, 4'-O-methylalpinumisoflavone by various techniques such as UV-Vis, ESI-MS, $^1H\;NMR$ and $^{13}C\;NMR$ spectroscopy. Finally, a method to characterize the compounds was developed by using the UPLC equipped with a $C_{18}$ column and a gradient mobile phase system consisting of 2% acetic acid in water (solvent A) and 2% acetic acid in methanol (solvent B). The developed method was validated with the parameters such as selectivity, linearity, limit of detection, limit of quantitation, accuracy, and precision, which are defined by the ICH (International Conference on Harmonization). Using the validated method, the compounds in the fruits harvested in different months were also quantitatively analyzed. We propose this approach this approach can readily be utilized as an efficient evaluation method to quantify the extracts of C. tricuspidata.

• Korean Journal of Pharmacognosy
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• v.47 no.1
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• pp.92-101
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• 2016

In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was established for simultaneous determination of the 25 marker components, including chlorogenic acid, gallic acid, oxypaeoniflorin, homogentisic acid, methyl gallate, caffeic acid, 3,4-dihydroxybenzaldehyde, paeoniflorin, albiflorin, liquiritin, nodakenin, ferulic acid, ginsenoside Rg1, liquiritigenin, coumarin, cinnamic acid, benzoylpaeoniflorin, ginsenoside Rb1, cinnamaldehyde, paeonol, glycyrrhizin, 6-gingerol, evodiamine, rutecarpine, and spicatoside A in traditional Korean formula, Onkyung-tang. All analytes were separated on 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 carried out using a Waters ACQUITY TQD LC-MS/MS coupled with an electrospray ionization (ESI) source in the positive and negative modes. The flow rate and injection volume were 0.3 mL/min and $2.0{\mu}L$, respectively. The correlation coefficient of all analytes in the test ranges was greater than 0.98. The limits of detection and quantification values of the 25 marker compounds were in the ranges 0.03-19.43 and 0.09-58.29 ng/mL, respectively. As a result, methyl gallate, 3,4-dihydroxybenzaldehyde, evodiamine, and rutecarpine were not detected in this sample and the concentrations of the 21 compounds except for the above 4 compounds were $33.09-3,496.32{\mu}g/g$ in Onkyung-tang decoction. Among these compounds, paeonol was detected at the highest amount as a $3,496.32{\mu}g/g$.

• Korean Journal of Environmental Agriculture
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• v.34 no.1
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• pp.52-56
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• 2015

BACKGROUND: Three commercial biopesticides containing derris extract, which is permitted as a commercial biopesticide substances by the Environmentally-friendly Agriculture Promotion Act, have been marketed in Korea. But, the quantitative analytical method of active substances for crop protection in biopesticides containing derris extract has not known. METHODS AND RESULTS: Solid phase extraction (SPE) cartridge clean-up method for the quantitative analysis of rotenone and deguelin in biopesticides containing derris extract was developed and validated by ultra-performance liquid chromatography (UPLC). The clean-up method was established using hydrophilic lipophilic balance (HLB) SPE cartridges for the bioactive substances in biopesticides containing derris extract, and the eluate was analyzed to quantify the rotenone and deguelin by the UPLC. LOQ and recovery rates of rotenone and deguelin were 0.085 and 0.044 mg/L, 95.7 and 93.3%, respectively. The content of rotenone and deguelin in three biopesticides containing derris extract were analyzed by the developed method, the results showed 0.001-0.236 and

• Food Science and Preservation
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• v.30 no.1
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• pp.28-41
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• 2023

Non-aflatoxigenic Aspergillus oryzae and aflatoxigenic A. flavus cannot be clearly identified by partial sequencing of the internal transcribed spacer (ITS) and 18S ribosomal ribonucleic acid (18S rRNA) regions. This study aimed to compare the accuracy among three aflatoxin detection methods using ultra-performance liquid chromatography (UPLC), high-performance liquid chromatography (HPLC), and an enzyme-linked immunosorbent assay (ELISA) kit and to select the non-aflatoxigenic Aspergillus sp. isolated from soybean paste. All analytical methods were suitable according to the international standards of Codex Alimentarius FAO-WHO (CODEX) or the Ministry of Food and Drug Safety (MFDS). UPLC exhibited the best of limit of detection (LOD) and limit of quantification (LOQ). Based on UPLC, HPLC, and the ELISA kit assay, the P5 and P7 strains isolated from soybean paste had 1,663.49, 1,468.12, and >20 ㎍/kg and 1,470.08, 1,056.73, and >20 ㎍/kg, respectively, detected and re-identified as A. flavus. In contrast, the P3 and P4 strains (A. oryzae), which were detected below the MFDS standards in all assays, were confirmed as non-aflatoxigenic fungi. Among the methods evaluated for quantitative analysis of aflatoxin, UPLC and HPLC are superior in terms of accuracy, and the ELISA kit rapidly detects low concentrations of aflatoxin. Furthermore, this study demonstrates that any Aspergillus sp. isolated for use as a fermentation starter should be analyzed for potential aflatoxin production using UPLC and HPLC for accurate quantitative analysis or ELISA for the rapid detection of low-level concentrations of aflatoxin.

• Natural Product Sciences
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• v.22 no.2
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• pp.93-101
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• 2016

For efficient quality control of the Samryeongbaekchul-san decoction, a powerful and accurate an ultra-performance liquid chromatography (UPLC) coupled with electrospray ionization (ESI) tandem mass spectrometry (MS) method was developed for quantitative analysis of the thirteen constituents: allantoin (1), spinosin (2), liquiritin (3), ginsenoside Rg1 (4), liquiritigenin (5), platycodin D2 (6), platycodin D (7), ginsenoside Rb1 (8), glycyrrhizin (9), 6-gingerol (10), atractylenolide III (11), atractylenolide II (12), and atractylenolide I (13). Separation of the compounds 1 - 13 was performed on a UPLC BEH $C_{18}$ column ($2.1{\times}100mm$, $1.7{\mu}m$) at a column temperature of $40^{\circ}C$ with a gradient solvent system of 0.1% (v/v) formic acid aqueous-acetonitrile. The flow rate and injection volume were 0.3 mL/min and $2.0{\mu}L$. Calibration curves of all compounds were showed good linearity with values of the correlation coefficient ${\geq}0.9920$ within the test ranges. The values of limits of detection and quantification for all analytes were 0.04 - 4.53 ng/mL and 0.13 - 13.60 ng/mL. The result of an experiment, compounds 2, 6, 12, and 13 were not detected while compounds 1, 3 - 5, and 7 - 11 were detected with 1,570.42, 5,239.85, 299.35, 318.88, 562.27, 340.87, 12,253.69, 73.80, and $115.01{\mu}g/g$, respectively.

• Korean Journal of Pharmacognosy
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• v.49 no.1
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• pp.70-75
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• 2018

Acer tegmentosum Maxim (ATM) has been used to treat hepatic disorders in traditional oriental medicine. However, there is little information about phytochemical constituents for quality control of ATM. In this study, we developed and established a simultaneous analytical method of the 10 marker compounds (three coumarins, 3 flavonoids, 1 lignan, 3 phenolics) in ATM using ultra-performance liquid chromatography-mass spectrometry (UPLC-MS/MS). Chromatographic separation of ten target analytes was achieved with a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$), using a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. Identifications and quantitation of all analytes were performed using a Q-Exactive UPLC-MS/MS system. Correlation coefficients of the calibration curve for all analytes were ${\geq}0.9986$. The values of limits of detection and quantification of all analytes were 0.5-10.0 and 5.0-50.0 ng/mL, respectively. The established UPLC-MS/MS method successfully identified all target analytes in ATM, and the phytochemicals were 0.01-67.98 mg/g in its lyophilized water extract.

• Proceedings of the Plant Resources Society of Korea Conference
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• 2010.05a
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• pp.5-5
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• 2010

Selection of specific medicinal sources as well as bioactive compounds is important for the preparation of medicine and related products with good quality. It is necessary to pay close attention for choosing correct medicinal sources, particularly in case of medicinal plants, because of their diversity, which can affect the quality and efficacy of medicine. Discrimination of plants based on morphological or genetic characteristics has been used as a conventional classification method of pharmaceutical sources so far; however, more need demands more general methods for accurate quality assessment of medicinal plants. In this study, ultra performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UPLC/Q-TOF MS) technique applied to this metabolic profiling is a powerful tool due to its higher sensitivity, resolution, and speed compared to conventional HPLC technique. The metabolite profiling of several medicinal plants including Panax ginseng was carried out using UPLC/Q-TOF MS and total metabolites were then subsequently applied to various statistical tools to compare the patterns. The developed metabolomics tool with UPLC/Q-TOF MS successfully identified and classified the samples tested according to their origins.