• The Korean Journal of Food And Nutrition
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• v.24 no.4
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• pp.617-621
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• 2011

$Coptis$ $chinensis$ Franch rhizome is one of the important traditional Korea medicines with anti-inflammatory, anti-bacterial, anti-hypertensive and anti-cancer properties. The methanol extract of rhizome from the $Coptis$ $chinensis$ rhizome was purified by using preparative centrifugal partition chromatography (CPC) and HPLC method. The optimum two-phase CPC solvent system was composed of n-butanol:acetic acid:water at a ratio of 4:1:5. Berberine (16.8 mg) was successfully isolated by CPC and HPLC. The chemical structure of the compound was identified by (1 H)$^1H$, $^{13}C$-NMR and ESI-MS spectral data analysis.

• Bulletin of the Korean Chemical Society
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• v.29 no.12
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• pp.2465-2470
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• 2008

• 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.

• Korean Journal of Veterinary Service
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• v.30 no.1
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• pp.1-12
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• 2007

A liquid chromatographic method has been developed for the analysis of aminoglycoside antibiotics (AMGs) using Heptafluorobutyric acid (HFBA) as a ion-pairing reagent. AMGs (amikacin, apramycin, dihydrostreptomycin, gentamicin, hygrosin B, kanamycin, neomycin, spectinomycin and tobramycin) were formed by reaction with HFBA as ion-pairing reagent. HFBA was attached to corresponding amino group of AMGs. These AMGs compounds were separated and detected by electrospray ionization mass spectrometry (ESI-MS). The experimental conditions for separation of AMGs were optimized and validated. A simple liquid chromatographic method for the determination of AMGs was demonstrated.

• Korean Journal of Food Science and Technology
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• v.42 no.4
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• pp.414-419
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• 2010

Hyphenated-HPLC techniques combine the separation power of HPLC with the structural and bioactivity information provided by NMR, ESI/MS, and an on-line antioxidant screening system. The major advantages over the traditional off-line techniques are rapidity and efficiency. In this study, we used hyphenated HPLC techniques including online HPLC-ABTS, LC-NMR, and LC-MS todirectly identify the major antioxidants of safflower (Carthamus tinctorius L.) seeds. The results demonstrated that the major antioxidant compounds from on-line HPLC-ABTS analysis were identified as 8'-hydroxyarcgenin-4'-O-$\beta$-D-glucoside, N-(p-coumaroyl) serotonin, and N-feruloylserotonin. Among them, N-feruloylserotonin accounted for almost 50% of the ABTS radical scavenging activity of the total extract. The results demonstrate that HPLC hyphenated techniques can be used to rapidly screen and structurally identify antioxidants from crude plant extracts.

• Analytical Science and Technology
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• v.22 no.4
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• pp.326-335
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• 2009

A specific analytical method able to identify and quantify traces of six glucocorticoids residues in eggs were developed. The extraction and clean-up parameters for simultaneous analysis were evaluated and HPLC and spectrometric conditions were also established. For determination of glucocorticoids, 5 g of egg was transferred into a test tube, adjusted pH 5.2 with acetate buffer and was $\beta$-glucuronidase/arylsulfatase from Helix pomatia added. The mixture was centrifuged and supernatant was extracted twice with 20 mL n-hexane. The extraction was performed with HLB cartridge using methanol, followed by clean-up with silica cartridge using methanol/ethyl acetate (4/6, v/v). The analytes were determined by HPLC/ESI-MS/MS operating in the negative ion mode. Validation studies with fortified egg samples for established method were performed. The result of method validation gave good efficiency, linearity, accuracy and precision. The correlation coefficients ($r^2$) of the calibration curves appeared to be higher than 0.99 in egg, indicating excellent linearity. LOD was ranged 0.09 to $0.17{\mu}g/kg$, and recoveries for most compounds were in the range of 55.7-69.8%. This method can be used to determine ${\mu}g/kg$ levels of glucocorticoids in eggs.

• Mass Spectrometry Letters
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• v.6 no.4
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• pp.99-104
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• 2015

A liquid chromatography mass spectrometry (LC-MS) system was used to identify and distinguish oligostilbene diastereoisomers. A polyphenolic extract from Neobalanocarpus heimii known to be rich in oligostilbenes of various degrees of condensation was used as test material. Fourteen oligostilbenes were isolated from this extract on a fully automated semi-preparative HPLC system. Out of these, two pairs of dimers, one pair of trimers, two pairs of tetramers and a group of four tetramers with similar skeleton were identified as diastereoisomers. Their structures and configurations were established by spectroscopic methods. All isolated compounds were subjected to an LC-MS/MS to study their fragmentation patterns. The experiments were performed on a liquid chromatography-mass spectrometry (LC-MS) with electrospray-ionization (ESI) interface in positive mode. MS/MS spectra of each pure compound were recorded by direct infusion in identical conditions and their product ion spectra were analysed. Some subtle yet significant differences were observed between the spectra of oligostilbenes from the various diastereoisomeric series.

• Natural Product Sciences
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• v.23 no.4
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• pp.247-252
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• 2017

The methylglyoxal (MGO) trapping constituents from onion (Allium cepa L.) peels were investigated using pre-column incubation of MGO and crude extract followed by HPLC analysis. The peak areas of MGO trapping compounds decreased, and their chemical structures were identified by HPLC-ESI/MS. Among major constituents in outer scale of onion, 2-(3,4-dihydroxybenzoyl)-2,4,6-trihydroxy-3(2H)-benzofuranone (2) was more effective MGO scavenger than quercetin (6) and its 4'-glucoside, spiraeoside (3). After 1 h incubation, compound 2 trapped over 90% MGO at a concentration of 0.5 mM under physiological conditions, but compounds 3 and 6 scavenged 45%, 16% MGO, respectively. HPLC-ESI/MS showed that compound 2 trapped two molecules of MGO to form a di-MGO adduct and compounds 3 and 6 captured one molecule of MGO to form mono-MGO adducts, and the positions 6 and 8 of the A ring of flavonoids were major active sites for trapping MGO.

• Mass Spectrometry Letters
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• v.10 no.4
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• pp.108-111
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• 2019

The hydrolysis of penicillin G, carbenicillin and ampicillin in pure water at room temperature was studied by high pressure liquid chromatography electrospray ionization mass spectrometry. Hydrolysis of ampicillin did not occur under these conditions; however, penicillin G and carbenicillin were completely hydrolyzed after seven days. A short interpretation of this difference is proposed. The mass spectrometric behaviour, namely ESI response and fragmentation pathway, of hydrolyzed penicillin G and hydrolyzed carbenicillin have been also discussed.

• Journal of Applied Biological Chemistry
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• v.65 no.3
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• pp.195-202
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• 2022

Soybean (Glycine max L.) leaves have been researched as functional food stuff actively, but there is no validation method to control quality of soybean leaves (SL). In this study, we annotated seven kaempferol derivatives to confirm camelliaside A as index metabolite in SL using UHPLC-ESI-TOF-MS. HPLC-UVD validation method of camelliaside A in hot-water extract of SL was established according to validation guideline of functional foods from the Ministry of Food and Safety of Korea. The HPLC-UVD method was validated with reliable parameters for examining specificity, accuracy, precision, limit of detection and quantification and linearity. The established method gave the suitable ranges to qunatitate camelliaside A from the hot-water extract of soybean leaves.