• Mass Spectrometry Letters
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• v.11 no.1
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• pp.10-14
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• 2020

Riboflavin is a water-soluble vitamin, which serves as a precursor to flavin mononucleotide and flavin adenine dinucleotide. This study aimed to develop a simple and rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis for the quantification of riboflavin in the Beagle dog plasma. This method utilized simple protein precipitation with acetonitrile and ¹³C₄, ¹⁵N₂-riboflavin was used as an internal standard (IS). For chromatographic separation, a hydrophilic interaction liquid chromatography (HILIC) column was used with gradient elution. The mobile phase consisted of 0.1% (v/v) aqueous formic acid with 10 mM ammonium formate and acetonitrile with 0.1% (v/v) formic acid. Since riboflavin is an endogenous compound, 4% bovine serum albumin in phosphate buffered saline was used as a surrogate matrix to prepare the calibration curve. The quantification limit for riboflavin in the Beagle dog plasma was 5 ng/mL. The method was fully validated for its specificity, sensitivity, accuracy and precision, recovery, and stability according to the US FDA guidance. The developed LC-MS/MS method may be useful for the in vivo pharmacokinetic studies of riboflavin.

• Food Science and Biotechnology
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• v.18 no.2
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• pp.561-564
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• 2009

A high performance liquid chromatography (HPLC) method has been developed for determination of 11 ginsenosides in black ginseng (BG, white ginseng that is subjected to 9 cycles of $95^{\circ}C$ for 3 hr). After eluted by gradient elution of water-acetonitrile without buffer in 70 min, 11 ginsenosides in BG were identified. The proposed method provided good linearity ($R^2$>0.9995), accuracy (92.2-106.6%), and intra- and interday precision (RSD<2.6%). In addition, ginsenosides compositions in white, red, and black ginsengs were investigated using this method, respectively. Interestingly, in BG, the content of ginsenoside $Rg_3$ which does not existed in white ginseng was 7.51 mg/g, approximately 20 times than that in red ginseng.

• KSBB Journal
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• v.15 no.6
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• pp.605-608
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• 2000

Oligodeoxynucleotides (ODNs) were separated by high-performance membrane chromatography (HPMC), a combined system of chromatography and membrane. The separation mechanism involved anion-exchange, and the stationary phase was cation CIM (Convective Interaction Media) DEAE disk (16${\times}$3 mm). Two types of mobile phase were used, buffer A (20mM Tris-HCl, pH 7.4) and buffer B (buffer A + 1M NaCl). As the amount of NaCl dissolved in buffer linearly increased, the retention time shortened, which enabled a gradient elution mode. Based on the number of theoretical plates and resolution observed, the optimum mobile phase and operating condition (Buffer A/Buffer B=50/50 - 20/80 vol%, gradient time 2 min) were experimentally determined. In this experimental condition, ODNs were separated within 2 min at a mobile phase flow rate of 6 ml/min.

• Bulletin of the Korean Chemical Society
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• v.30 no.1
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• pp.61-66
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• 2009

An analytical method based on solid-phase extraction and gas chromatography / mass spectrometry has been developed for measurement of acaricides (amitraz, bromopropylate, coumaphos, cymiazole, and tetradifon) in honey sample. In the stability test of acaricides in honey, amitraz underwent a rapid degradation into 2,4-dimethylaniline (DMA), 2,4-dimethylphenylformamide (DMPF), and N-(2,4-dimethylphenyl)-N'-methylformamidine (DMPMF), whileas other acaricides were found to be stable even for over three months. Extraction of five acaricides from 5g of honey sample was carried out by liquid-liquid extraction using 20mL of ethylacetate. For purification, Florisil-SPE cartridge with elution of 5mL of n-hexane/ acetone (55:45, v/v) was found to remove interferences effectively. Quantification was performed using gas chromatography / mass spectrometry in the selected ion monitoring mode. Spiking experiments were carried out to determine the recovery, precision, and limits of detection (LODs) of the method. The overall recovery values from honey spiked at 0.02 and 0.20 ${\mu}g/g$ levels, respectively, were found to be greater than 75% for all acaricides. The method detection limits for acaricides were ranged from 0.1 to 3 ppb. The developed method in this study was applied for the monitoring of acaricides in honey products collected from urban markets in Korea.

• Biotechnology and Bioprocess Engineering:BBE
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• v.9 no.6
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• pp.495-499
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• 2004

The analyses of peak shapes in chromatography are useful in operating chroma­tographic system. The asymmetry and sharpness of a chromatographic peak are estimated by the reversed-phase adsorption of two standard peptides (angiotensin II bradykinin) on $C_{18}$ In this work, the average particle diameters of $C_{18}$ were 5 and 15 $\mu$m, while the pore sizes were 100 and 300 A. The composition of the mobile phase was $50/50\;vol.\;{\%}$ of a binary mixture of acetonitrile and water with $0.1\%$ TFA, and the particles were packed in a stainless column ($4.6{\times}150$ mm). The third and the fourth central movement were calculated from the chromatographic elution curves by moment analysis. The peak asymmetry was determined by two theoretical calculations: the asymmetry factor by elution peak analysis and skewness with moment analysis. The sharpness was estimated by the fourth central moment. In this work, the most acceptable skewness was calculated when the pore size was 300 A. The large excess was observed on small pore size.

• Journal of the Korean Chemical Society
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• v.29 no.4
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• pp.419-425
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• 1985

N-Methylamidinoglycine, an isomer of creatine which was postulated to be formed enzymatically in vitro, has been synthesized by coupling glycine with N, S-dimethylthiopseudouronium iodide in a yield of approxirnately 60%. On heating in acidic solution, it was converted to a cyclized form (isocreatinine) in analogy with the conversion of creatine to creatinine(anhydrous form). Structures were confirmed by an elemental analysis and proton NMR spectroscopy. Further studies on their characteristics were compared with those of creatine and creatinine in regard to isoelectric points(pI), retardation coefficients(Rf) on thin layer chromatography, and elution profiles on amino acid analyzer. In order to facilitate the comparison, $^{14}C$-labeled creatine, creatinine, isocreatine and isocreatinine were also synthesized.

• Analytical Science and Technology
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• v.6 no.4
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• pp.383-390
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• 1993

Retention behaviors of aliphatic and aromatic compounds were investigated with Van der Waals volume which represented the molecular size. The organic solvents, methanol, acetonitrile and tetrahydrofuran, were mixed with water at various ratio, respectively. The selectivity of organic solvents were tested by change of column temperature. The capacity factor was increased linearly according to the enlargement of molecular size. Therefore, Van der Waals volume was useful to predict the elution of organic molecules in reversed-phase column. The order of elution capacity of solvents was methanol

• Applied Biological Chemistry
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• v.35 no.3
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• pp.196-201
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• 1992

Characteristics on lintnerization of dry type (Suwon 147) and moist type (Hwangmi) sweet potato starches were investigated. Chain distribution of lintnerized starches was also studied by debranching with pullulanase. Hydrolytic patterns of two starches showed two distinct stages and hydrolysis extents of Suwon 147 starch were lower than those of Hwangmi starch. The relative crystallinities of Suwon 147 starches were higher than those of Hwangmi starch. The elution profiles of lintnerized starches were composed of two peaks about degree of polymerization (DP) 25 and DP 15. The elution profiles of debranched samples showed only one peak about DP 15 and peak DP of Suwon 147 lintnerized starch was higher than that of Hwangmi.

• Korean Journal of Medicinal Crop Science
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• v.15 no.3
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• pp.215-219
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• 2007

This study was conducted to analyze not only for the quality guaranteed of red ginseng but also for the minor ginsenosides. Although several studies have reported to analyze ginseng saponins, those were focused to major saponins, including 6 to 7 ginsenosides. As increase of interest in medicinal effect of ginseng products, anasis of various ginsenosides in both red and white ginseng are strongly demanded. To perform optital condition of 12 ginsenoside analysis, We controlled HPLC conditions, such as the gradient elution of the mobile phase. We found the adequate separation method for 12 ginse-nosides. The optimum condition was as following : H$_2$O/CH$_3$CN ratios were 82/18, 70/30, 55/45 and 50/50, respectively. Sol-vent flow rate was 1.00 ma/min. Column temperature was kept to 35$^{\circ}$C. UV detector was set to 203 nm.

• Restorative Dentistry and Endodontics
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• v.23 no.1
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• pp.379-390
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• 1998

In endodontic treatment, calcium hydroxide has been used as intracanal medicament. Although calcium hydroxide should be removed thoroughly before permanent root canal filling, no effective method for its removal has been reported. Because of irregularity of root canal walls, root curvatures and anatomic variations, it is insufficient to remove calcium hydroxide from the canal wall only by mechanical instrumentation Considering the chemical effects of irrigants on calcium hydroxide, $Ca^{++}$ dissolving effect from two calcium hydroxide products is investigated, using dis- tilled water, NaOCl, citric acid and EDTA. Vitapex$^{(R)}$ 0.1g and calcium hydroxide 0.03g were dissolved in distilled water, 5% NaOCl, 50% citric acid and 17% EDTA respectively, at 1, 3, 5, 10min. time interval. The solution was filtered using filter paper(pore size $5{\mu}m$) and $Ca^{++}$ concentration was determined by ion chromatography. The result were as follows : 1. Distilled water, NaOCl, citric acid and EDTA abstracted more $Ca^{++}$ from calcium hydroxide than Vitapex$^{(R)}$ except NaOCl 1, 5, 10 time interval. 2. EDTA and citric acid abstracted more $Ca^{++}$ from Vitapex$^{(R)}$ and calcium hydroxide than distilled water or NaOCl. The overall result support the view that water-based calcium hydroxide product is easily removed than oil-based calcium hydroxide product and EDTA, citric acid are more effective in $Ca^{++}$ elution than NaOCl or distilled water.