• Korean Journal of Pharmacognosy
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• v.48 no.4
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• pp.320-328
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• 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 $548.13{\mu}g/g$.

• Bulletin of the Korean Chemical Society
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• v.34 no.9
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• pp.2663-2670
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• 2013

The purpose of stability testing is to provide evidence about how the quality of a drug varies with time under the influence of a variety of environmental factors. In this study, erythropoietin (EPO) was analyzed under different pH (pH 3 and pH 9) and temperature ($25^{\circ}C$ and $40^{\circ}C$) conditions according to current Good Manufacturing Practice (cGMP) and International Conference on Harmonisation (ICH) guidelines. The molecular weight difference between intact EPO and deglycosylated EPO was determined by SDS-PAGE, and aggregated forms of EPO under thermal stress and high-pH conditions were investigated by size exclusion chromatography. High pH and high temperature induced increases in dimer and high molecular weight aggregate forms of EPO. UPLC-ESI-TOF-MS was applied to analyze the changed modification sites on EPO. Further, normal-phase high-performance liquid chromatography was performed to identify proposed glycan structures and high pH anion exchange chromatography was carried out to investigate any change in carbohydrate composition. The results demonstrated that there were no changes in modification sites or the glycan structure under severe conditions; however, the number of dimers and aggregates increased at $40^{\circ}C$ and pH 9, respectively.

• ALGAE
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• v.39 no.3
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• pp.187-205
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• 2024

Chlorella species of microalgae are utilized in the crop and food industries. The aim of this research was to investigate the metabolite profiles of Chlorella fusca for the first time and evaluate its biological properties. The two ion modes of UPLC-Q-TOF-MS/MS were used to identify a total of 62 components in the methanol extract of C. fusca, with 26 in the negative and 36 in the positive ion mode, including 10 identical ingredients. Fatty acids (negative mode) and combinations of chlorophyll and fatty acids (positive mode) were the most prevalent chemical structures, constituting over 80 and 70% of the total metabolites, respectively, followed by chlorophyll, polar lipids, carotenoids, and fatty alcohols. Moreover, this extract exhibited potent antioxidant and anti-aging benefits in decreasing order of potency at a concentration of 200 ㎍ mL^-1: tyrosinase inhibition (100%), ABTS radical scavenging (90%), elastase inhibition (88%), and DPPH radical scavenging (34%). Notably, this extract protected the mobility of DNA fragments up to 5 ㎍ mL^-1 (26%), with potential effects (> 60% at 200 ㎍ mL^-1). These findings suggest that C. fusca may be a promising candidate for applications related to its biological functions, owing to the high accumulation of fatty acids and chlorophyll derivatives.

• 한국약용작물학회:학술대회논문집
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• 2008.11a
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• pp.477-478
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• 2008

• International Journal of Industrial Entomology and Biomaterials
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• v.37 no.2
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• pp.43-48
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• 2018

Mulberry fruit is a new income product in Korea sericulture due to the increase of fruit consumption. However, flavonoids of Korean mulberry cultivar for fruit production did not reported yet. In this study, the typical mulberry cultivar, 'Daeshim' was analyzed using ultrahigh performance liquid chromatography coupled with diode array detection and quadrupole time-of-flight mass spectrometry (UPLC-DAD-QTOF/MS) technique for flavonoids analysis. Nine flavonoids were isolated and analyzed from Daeshim using UPLC-DAD-QTOF/MS chromatogram. According to quantitative analysis, rutin (66.1 mg/100g DW) and quercetin 3-O-(6"-O-malonyl) glucoside (26.7 mg/100g DW) were abundant in mulberry fruit. Our results might be used as basic information for mulberry consumption.

• Analytical Science and Technology
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• v.30 no.6
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• pp.379-389
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• 2017

In this study, we set up an analytical method that can be used for rapid and accurate determination of representative isoquinoline alkaloids in medicinal plants using UPLC-ESI-Q-TOF MS (ultra pressure liquid chromatography-electrospray ionization-quadrupole-time-of-flight mass spectrometry). The compounds were eluted on a C18 column with 0.1 % formic acid and acetonitrile, and separated with good resolution within 13 min. Each of the separated components was characterized by precursor ions (generated by ESI-Q-TOF) and fragment ions (produced by collision-induced dissociation, CID), which were used as a reliable database. We also performed method validation: analytes showed excellent linearity ($R^2$, 0.9971-0.9996), LOD (5-25 ng/mL), LOQ (17-82 ng/mL), accuracy (91.6-97.4 %) as well as intra- and inter-day precisions (RSD, 1.8-3.2 %). In the analysis of Chelidonium majus L., magnoflorine, coptisine, sanguinarine, berberine and palmatine were detected by matching retention times and characteristic fragment ion patterns of reference standards. We also confirmed that, among the quantified components, coptisine was present in the highest quantity. Furthermore, alkaloid profiling was carried out by analyzing the fragment ion patterns corresponding to peaks of unknown components. In this manner, protopine, chelidonine, stylopine, dihydroberberine, canadine, and nitidine were tentatively identified. We also proposed the molecular structure of the fragment ions that appear in the mass spectrum. Therefore, we concluded that our suggested method for the determination of major isoquinoline alkaloids by UPLC-Q-TOF can be useful not only for quality control, but also for rapid and accurate investigation of phytochemical constituents of medicinal plants.

• Journal of Applied Biological Chemistry
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• v.63 no.4
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• pp.393-399
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• 2020

Saposhnikoviae Radix (SR) and Peucedani Japonici Radix (PR) have been used as the main traditional herbal medicines in Korea, China and Japan. In this study, ultra-performance liquid chromatography coupled to quadrupole time of flight mass spectrometry (UPLC-QTOF/MS)-based metabolomics was applied to evaluate the quality of SR and PR using the marker compounds. In the S-plot of SR and PR, 5-O-methylvisammioside and peucedanol were selected as a marker compound for SR and PR, respectively. Also, an UPLC method was established and well validated for marker compounds of SR and PR. These results suggested that the established analysis method could be used one of the good methods for the classification and quality assessment of SR and PR.

• 한국약용작물학회:학술대회논문집
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• 2011.09a
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• pp.90-91
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• 2011

• 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.

• Herbal Formula Science
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• v.21 no.1
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• pp.177-185
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• 2013

Objectives : Leejung-tang (Lizhong-tang) has been used for treatment of gastrointestinal disorders in Korea. In this study, we performed quantification analysis of five marker components, liquiritin, ginsenoside Rb1, ginsenoside Rg1, glycyrrhizin, and 6-gingerol in Leejung-tang using a ultra performance liquid chromatography- electrospray ionization-mass spectrometer (UPLC-ESI-MS). In addition, we evaluated antioxidant activity of Leejung- tang. Methods : The column for separation of five constituents used a UPLC BEH C18 ($100{\times}2.1mm$, $1.7{\mu}m$) maintained at $45^{\circ}C$. The mobile phase consisted of two solvent systems, 0.1% (v/v) formic acid in H2O (A) and CH3CN (B) by gradient flow. The flow rate was 0.3 mL/min with detection at mass spectrometer. The antioxidative activities conduct an experiment on 2,2'-azinobis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) and 2,2-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging activities of Leejung-tang. Results : Calibration curves of five marker compounds were acquired with r2 values > 0.99. The amount of the five compounds in Leejung-tang were 0.07 - 0.84 mg/g. The concentration required for 50% reduction (RC50) against ABTS radical was 119.02 ug/mL. In addition, the scavenging against DPPH radical of Leejung-tang was 11.4%, 14.5%, 19.8%, 29.6%, and 49.2% at 25 ug/mL, $50{\mu}g/mL$, $100{\mu}g/mL$, $200{\mu}g/mL$, and $400{\mu}g/mL$, respectively. Conclusions : The established LC-MS/MS method will be helpful to improve quality control of Leejung-tang. In addition, Leejung-tang is a potential antioxidant therapeutic agent.