• Journal of Biomedical and Translational Research
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• v.19 no.4
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• pp.130-139
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• 2018

This study aimed to analyze a high-performance liquid chromatography (HPLC) separation using a pentafluorophenyl column of parent drug hydroxychloroquine (HCQ) and its active metabolite, desethylhydroxchloroquine (DHCQ) applying to determine bioequivalence of two different formulations administered to patients. A rapid, simple, sensitive and specific liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for bioanalysis of HCQ and its metabolite DHCQ in human whole blood using deuterium derivative $hydroxychloroquine-D_4$ as an internal standard (IS). A triple-quadrupole mass spectrometer was operated using electrospray ionization in multiple reaction monitoring (MRM) mode. Sample preparation involves a two-step precipitation of protein techniques. The removed protein blood samples were chromatographed on a pentafluorophenyl (PFP) column ($50mm{\times}4.6mm$, $2.6{\mu}m$) with a mobile phase (ammonium formate solution containing dilute formic acid) in an isocratic mode at a flow rate of 0.45 mL/min. The standard curves were found to be linear in the range of 2 - 500 ng/mL for HCQ; 2 - 2,000 ng/mL for DHCQ in spite of lacking a highly sensitive MS spectrometry system. Results of intra- and inter-day precision and accuracy were within acceptable limits. A run time of 2.2 min for HCQ and 2.03 min for DHCQ in blood sample facilitated the analysis of more than 300 human whole blood samples per day. Taken together, we concluded that the assay developed herein represents a highly qualified technology for the quantification of HCQ in human whole blood for a parallel design bioequivalence study in a healthy male.

• Mass Spectrometry Letters
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• v.12 no.2
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• pp.53-58
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• 2021

Previous in vitro studies have demonstrated that ginsenoside Rc inhibits UGT1A9, but there are no available data to indicate that ginsenoside Rc inhibits UGT1A9 in vivo. The effect of single and repeated intravenous injection of ginsenoside Rc was evaluated on the pharmacokinetics of mycophenolic acid. After injection of ginsenoside Rc (5 mg/kg for one day or 3 mg/kg for five days), 2-mg mycophenolic acid was intravenously injected, and the pharmacokinetics of mycophenolic acid and mycophenolic acid-β-glucuronide were determined. Concentrations of mycophenolic acid and its metabolite from rat plasma were analyzed using a liquid chromatography-triple quadrupole mass spectrometry. Single or repeated pretreatment with ginsenoside Rc had no significant effects on the pharmacokinetics of mycophenolic acid (P > 0.05): The mean difference in maximum plasma concentration (C_max) and area under the concentration-time curve (AUC_inf) were within 0.83- and 0.62-fold, respectively, compared with those in the absence of the ginsenoside Rc. These results indicate that ginsenoside Rc has a negligible effect on the disposition of mycophenolic acid in vivo despite in vitro findings indicating that ginsenoside Rc is a selective UGT1A9 inhibitor. As a result, ginsenoside Rc has little possibility of interacting with drugs that are metabolized by UGT1A9, including mycophenolic acid.

• 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.

• Mass Spectrometry Letters
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• v.12 no.1
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• pp.1-10
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• 2021

A simple, specific, and economical LC-MS/MS method was investigated for the screening of 43 prescribed antihypertensive and related drugs in human urine. The urine samples were simply prepared by diluting and mixing with internal standard before directly introduced to the LC-MS/MS system, which is fast, straightforward, and cost-effective. Fractional factorial, Box-Behnken, and I-optimal design were applied to screen and optimize the mass spectrometric and chromatographic factors. The analysis was carried out on a triple quadrupole mass spectrometer system utilizing multiple reaction monitoring with positive and negative electrospray ionization method. Chromatographic separation was performed on a Thermo Scientific Accucore RP-MS column (50 × 3.0 mm ID., 2.6 ㎛) using two separate gradient elution programs established with the same mobile phases. Chromatographic separation was performed within 12 min. The optimal method was validated based on FDA guideline. The results indicated that the assay was specific, reproducible, and sensitive with the limit of detection from 0.1 to 50.0 ㎍/L. The method was linear for all analytes with coefficient of determination ranging from 0.9870 to 0.9981. The intra-assay precision was from 1.44 to 19.87% and the inter-assay precision was between 2.69 and 18.54% with the recovery rate ranges from 84.54 to 119.78% for all drugs measured. All analytes in urine samples were stable for 24 h at 25℃, and for 2 weeks at -60℃. The developed method improves on currently existing methods by including larger number of cardiovascular medications and better sensitivity of 12 analytes.

• Fashion & Textile Research Journal
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• v.23 no.6
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• pp.844-851
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• 2021

Due to the increase in consumers' interest about well-being, interest in eco-friendly products has been increasing due to the harmful effects of various harmful substances contained in textile products and environmental issues. As a result, natural dyes of less potential risk than synthetic dyes and digital textile printing(DTP) textile products with less environmental pollution are drawing attention. However, due to the lack of evaluation criteria for DTP textile products with natural ink and the nature of many colors are stacked layer by layer for dying, the need for simultaneous analysis is emerging. To evaluate whether the natural dye is derived from natural ingredients, the biocarbon content is analyzed. However, in the case of ink made using natural dyes and DTP textile products using natural ink, it is difficult to analyze the biocarbon content due to the limitation of the presence of a small amount of dye contained therein. In this study, we were shown the possibility of natural derived verification by cross-checking the analytes of natural dyes (Persicaria tinctoria, an indigo dye; Dactylopius coccus, a light red; and Curcum longa L., i.e., turmeric) and natural ink with HPLC-MS/MS. The coefficient of determination was 0.999 or higher, the limit of quantification was 0.647-3.664 ㎍/L and a %RSD of each indicator material was less than 10. Then, the extraction amount of natural dyes for five patterned fabrics was analyzed.

• Journal of Ginseng Research
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• v.46 no.2
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• pp.290-295
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• 2022

Background: Dried and red ginseng are well-known types of processed ginseng and are widely used as healthy food. The dried and red ginseng quality may vary with the storage period of raw ginseng. Therefore, herein, the effect of the storage period of fresh ginseng on processed ginseng quality was evaluated through multicomponent quantification with statistical analysis. Methods: A method based on ultrahigh performance liquid chromatography coupled to triple quadrupole mass spectrometry in multiple-reaction monitoring mode (UPLC-MRM-MS) was developed for quantitation of ginsenosides and oligosaccharides in dried and red ginseng. Principal component analysis and partial least squares discriminant analysis were conducted to evaluate the dynamic distributions of ginsenosides and oligosaccharides after different storage periods. Results: Eighteen PPD, PPT and OLE ginsenosides and nine reducing and nonreducing oligosaccharides were identified and quantified. With storage period extension, the ginsenoside content in the processed ginseng increased slightly in the first 2 weeks and decreased gradually in the following 9 weeks. The content of reducing oligosaccharides decreased continuously as storage time extending, while that of the nonreducing oligosaccharides increased. Chemical conversions occurred during storage, based on which potential chemical markers for the storage period evaluation of fresh ginseng were screened. Conclusion: According to ginsenoside and oligosaccharide distributions, it was found that the optimal storage period was 2 weeks and that the storage period of fresh ginseng should not exceed 4 weeks at 0 ℃. This study provides deep insights into the quality control of processed ginseng and comprehensive factors for storage of raw ginseng.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 1999.10a
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• pp.59-59
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• 1999

In this study, planer inductively coupled $Cl_2$ based plasmas were used to etch InGaN and the effects of plasma conditions on the InGaN etch properties have been characterized using quadrupole mass spectrometry(QMS) and optical emission spectroscopy(OES). As process conditions used to study the effects of plasma characteristics on the InGaN etch properties, $Cl_2$ was used as the main etch gas and $CHF_3,{\;}CH_4$, and Ar were used as additive gases. Operational pressure was varied from SmTorr to 3OmTorr, inductive power and bias voltage were varied from 400W to 800W and -50V to -250V, respectively while the substrate temperature was fixed at 50 centigrade. For the $Cl_2$ plasmas, selective etching of GaN to InGaN was obtained regardless of plasma conditions. The small addition of $CHF_3$ or Ar to $Cl_2$ and the decrease of pressure generally increased InGaN etch rates. The selective etching of InGaN to GaN could be obtained by the reduction of pressure to l5mTorr in $CI_2/IO%CHF_3{\;}or{\;}CI_2/IO%Ar$ plasma. The enhancement of InGaN etch rates was related to the ion bombardment for $CI_2/Ar$ plasmas and the formation of $CH_x$ radicals for $CI_2/CHF_3(CH_4)$ plasmas.

• Natural Product Sciences
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• v.28 no.4
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• pp.168-180
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• 2022

Ephedra is a genus of the Ephedraceae family and is found in temperate regions, such as Central Asia and Europe. Among the various ephedra species, Ma Huang (Ephedra herb) is derived from the aerial parts of Ephedra sinica S tapf, Ephedra equisetina Bunge, and Ephedra intermedia Schrenk & C.A. Mey. Ma Huang contains various ephedra alkaloids, including (-)-ephedrine, (+)-pseudoephedrine, (-)-norephedrine, (+)-norpseudoephedrine, (-)-methylephedrine, and (+)-methylpseudoephedrine, which are found naturally as single enantiomers, although they can be prepared as racemates. Although the use of Ma Huang in foods is prohibited in Korea, products containing Ma Huang can be imported, and so it is necessary to develop a suitable analytical technique for the detection of Ma Huang in foods. Herein, we report the development of analytical methods for the detection of ephedra alkaloids in products containing Ma Huang. Following sample purification by solid phase extraction, quantitative analysis was performed using ultra-performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS). Additionally, the enantiomers were successfully separated using HPLC-DAD. We successfully analyzed various food samples, where the ephedra alkaloids were qualitatively and quantitatively determined, and the enantiomers were separated. It is expected that these methods may contribute toward preventing the distribution of illegal products containing Ma Huang.

• Analytical Science and Technology
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• v.36 no.1
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• pp.22-31
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• 2023

As the use of e-liquid cigarettes is rapidly increasing worldwide, it multiplies the potential risk undisclosed to the health of non- and smokers. To reduce the hazard, each country has its own set of regulations for controlling e-liquids. In Korea, the narrow definition of tobacco makes it difficult and have been steadily occurring tax evasion exploiting the difference in natural and artificial nicotine. Therefore, it is very important to distinguish source of nicotine for their regulation. To find biochemical discriminant markers, this study established analysis methods based on high-performance liquid chromatography coupled with diode array detector (HPLC-DAD) and high-performance liquid chromatography coupled with triple Quadrupole mass spectrometry (HPLC-MS/MS) for nicotine enantiomers and tobacco alkaloids targeted using the difference in pathways of nicotine biosynthesis and chemical synthesis. The method was validated by experimenting linearity (R² > 0.999), recovery (80.99-108.41 %), accuracy (94.11-109.73 %) and precision (0.04-8.27 %). Then, the results for discrimination of the nicotine obtained from analysis of 65 commercial e-liquid products available in Korean market was evaluated. The method successfully applied to the e-liquids and one sample labelled 'synthetic nicotine' for tax exemption was found to contain a natural nicotine product. This method can be used to determine whether an e-liquid product uses natural or artificial nicotine and monitor non-taxable e-liquid products. The method is more scientific than the existing one, which relies only on field evidence.

• The Korean Journal of Food And Nutrition
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• v.36 no.6
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• pp.543-550
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• 2023

Mulberry fruit is a superior source of polyphenols, especially anthocyanin, and has a long history of use as an edible fruit and traditional medicine. The anthocyanin composition of mulberry fruit from 15 Korean cultivars was analyzed by ultra-performance liquid chromatography diode array detector with quadrupole time of flight/mass spectrometry (UPLC-DAD-QToF/MS) based on a cyanin internal standard. The four glycosides were identified by comparison with authentic standards and published reports. The major anthocyanin was cyanidin 3-O-glucoside (71.7%), followed by cyanidin 3-O-rutinoside (26.6%). The minor components (total of 1.7%) were pelargonidin 3-O-glucoside and pelargonidin 3-O-rutinoside. The total anthocyanin content (mg/100 g, dry weight) of mulberry fruit varied by cultivar and ranged from 471.5±4.0 (Su Hong) to 4,700.2±54.0 (Gwa Sang2). Among the 15 cultivars examined, Gwa Sang2 showed the highest level of cyanidin 3-O-glucoside (3,133.4±32.6), which was 9-fold higher than that of Su Hong (351.5±3.4). In conclusion, anthocyanin profiles, including pelargonidin 3-O-glucoside and pelargonidin 3-O-rutinoside, were reported for the first time from 15 Korean mulberry fruit cultivars. The results will contribute valuable information on pharmaceutical properties, breeding superior mulberry cultivars, and food industries.