• Natural Product Sciences
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• v.26 no.1
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• pp.64-70
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• 2020

Citrus junos seeds (CS) have been traditionally used for the treatment of cancer and neuralgia. They are also used to manufacture edible oil and cosmetic perfume. A large amount of CS shells without oil (CSS) are discarded after the oil in CS is used as foods or herbal remedy. To efficiently utilize CSS as a by-products, it needs to be studied through chemical analysis. Therefore, we developed an ultra-performance liquid chromatography (UPLC)-diode array detection (DAD) method for simultaneous determination and quantitative analysis of five components (two flavonoids and threes limonoids) in CSS. A Waters Acquity UPLC HSS T3 column C18 (2.1 × 100 mm, 1.8 ㎛) was used for this separation. It was maintained at 40 ℃. The mobile phase used for the analysis was distilled water and acetonitrile with gradient elution. To identify the quantity of the five components, a mass spectrometer (MS) with an electrospray ionization (ESI) source was used. The regression equation showed great linearity, with correlation coefficient ≥ 0.9912. Limits of detection (LOD) and limits of quantification (LOQ) of the five compounds were 0.09 - 0.13 and 0.26 - 0.38 ㎍/mL, respectively. Recoveries of extraction ranged from 97.45% to 101.91%. Relative standard deviation (RSD) values of intra- and inter-day precision were 0.06 - 1.15% and 0.19 - 0.25%, respectively. This UPLC-DAD method can be validated to simultaneously analyze quantities of marker flavonoids and limonoids in CSS.

• The Korean Journal of Food And Nutrition
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• v.32 no.6
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• pp.717-729
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• 2019

The chemical informs about 70 individual phenolic compounds were constructed from various lettuce samples based on literature sources and analytical data. A total of 30 phenolic compounds including quercetin 3-O-glucuronide, quercetin 3-O-(6''-O- malonyl) glucoside, cyanidin 3-O-(6''-O-malonyl)glucoside, chlorogenic acid and chicoric acid as major components were identified in 6 lettuce samples from Korea using UPLC-DAD-QToF/MS on the basis of constructed library. Among these, quercetin 3,7-di-O-glucoside(m/z 627 [M+H]⁺), quercetin 3-O-(2''-O-malonyl)glucoside(morkotin C, m/z 551 [M+H]⁺), quercetin 3-O-(6''- O-malonyl)glucoside methyl ester(m/z 565 [M+H]⁺), 5-O-cis-p-coumaroylquinic acid(m/z 339 [M+H]⁺) and 5-O-caffeoylquinic acid methyl ester(m/z 369 [M+H]⁺) were newly confirmed from the lettuce samples. In total content of phenolic compounds, 4 red lettuce samples(2,947.7~7,535.6 mg/100 g, dry weight) showed higher than green lettuce(2,687.3 mg) and head lettuce(320.1 mg).

• Korean Journal of Pharmacognosy
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• v.47 no.4
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• pp.366-373
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• 2016

Bulhwangeumjeonggisan (BHGJGS) is a traditional herbal formulation generally used in the treatment of cold and gastritis. BHGJGS consists of eight herbal plants; Atractylodis Rhizoma, Magnoliae Cortex, Citri Pericarpium, Glycyrrhizae Radix, Agastachis Herba, Pinelliae Rhizoma, Zingiberis Rhizoma and Zizyphi Fructus. Complete standardization of this formulation has not been done yet. So, a simple and accurate method was developed and validated using Ultra Performance Liquid Chromatography (UPLC) with Diode Array Detector (DAD) for the standardization of BHGJGS. UPLC conditions were optimized using a c18 RP-Amide column with mobile phase; 0.1% phosphate buffer and acetonitrile, detection wavelength; 210 and 325 nm. The linearities of calibration curves were acceptable ($R^2$>0.9994), and the limit of detection and quantification were within the ranges of 0.011-0.091 and $0.034-0.277{\mu}g/ml$ respectively. The relative standard deviation (RSD) of intra- and inter-day precisions were under 3.61%. The RSD of repeatability was under 0.68 %. The results of recovery test were 94.4-107.9%, and the RSD were under 4.6%. The developed method was used to find the contents of standard constituents in BHGJGS mix extract powder, and two commercial formulation (A and B). The data show that the developed method was specific, sensitive, accurate, and precise for analysis of BHGJGS components.

• 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.

• Journal of Ginseng Research
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• v.40 no.4
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• pp.382-394
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• 2016

Background: Ginsenosides are the characteristic and principal components which manifest a variety of the biological and pharmacological activities of the roots and rhizomes of Panax ginseng (GRR). This study was carried out to qualitatively and quantitatively determine the ginsenosides in the cultivated and forest GRR. Methods: A rapid and sensitive ultra-high-performance liquid chromatography coupled with diode-array detector and quadrupole/time of flight tandem mass spectrometry (UPLC-DAD-QTOF-MS/MS) was applied to the qualitative analysis of ginsenosides and a 4000 QTRAP triple quadrupole tandem mass spectrometer (HPLC-ESI-MS) was applied to quantitative analysis of 19 ginsenosides. Results: In the qualitative analysis, all ingredients were separated in 10 min. A total of 131 ginsenosides were detected in cultivated and forest GRR. The method for the quantitative determination was validated for linearity, precision, and limits of detection and quantification. 19 representative ginsenosides were quantitated. The total content of all 19 ginsenosides in the forest GRR were much higher than those in the cultivated GRR, and were increased with the growing ages. Conclusion: This newly developed analysis method could be applied to the quality assessment of GRR as well as the distinction between cultivated and forest GRR.

• 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.

• Korean Journal of Environmental Agriculture
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• v.36 no.4
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• pp.249-255
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• 2017

BACKGROUND: Globally, mulberry (Morus sp.) is exploited for feeding leaf to silkworms in order to obtain silk fiber or for animal feedstock production. Also, mulberry fruit is known to a by-product that was produced from mulberry tree after harvesting leaves for silkworm rearing, as a yield and consumption of mulberry fruit was increased, it has been fixing to a newincome crop. Mulberry leaves and fruits are used for the health benefits of human beings. Mulberry contains various bioactive components, such as alkaloids and flavonoids. Mulberry flavonoids are an important part of the diet because of their effects on human nutrition. The flavonoids in mulberry leaf and fruit of 'Suhyang'(Morus alba L.) were determined. METHODS AND RESULTS: Flavonoids for mulberry leaf and fruit of 'Suhyang' were analysed using ultrahigh performance liquid chromatography coupled with diode array detection and quadrupole time-of-flight mass spectrometry (UPLC-DAD-QTOF/MS)technique. An UPLC-DAD-QTOF/MS system was used, and identification of mulberry leaves constituents was carried out on the basis of the complementary information obtained from LC spectra, MS ions, and MS/MS fragments. The mulberry leaf (16 flavonoids) and fruit (9 flavonoids) were isolated and analyzed from Suhyang using UPLC-DAD-QTOF/MS chromatogram. To the best of our knowledge, Quercetin 3-O-(6"-O-malonyl) glucoside and quercetin 3-O-rutinoside (rutin) was detected on the highest content in leaf and fruit, respectively and further research will be devoted to evaluate their biological activity. CONCLUSION: Obtaining information about the concentration of functional materials in mulberry leaves could contribute to the development and promotion of processed, functional products and offer possible industrial use of 'Suhyang', holding promises to enhance the overall profitability of sericulture.

• Food Science and Preservation
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• v.23 no.7
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• pp.1004-1011
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• 2016

Flavonoids, non-nutrient secondary metabolites of plants, are widely distributed in commonly consumed agro-food resources. Flavonoids include aglycones, and their glycosides are reported to have potential health-promoting compounds. The aim of this study was to investigate flavonoid glycosides in the fruit and leaves of Zizyphus jujuba var. inermis (Bunge) Rehder (jujube). A total of six flavonoids (five flavonols and one chalcone) were identified in jujube fruit and leaves by using ultra-performance liquid chromatography-diode array detector-quadrupole time of flight mass spectrometry along with chemical library and an internal standard. In positive ion mode, six flavonoids were linked to the C- and O-glycosides which were conjugated with sugar moieties based on kaempferol, quercetin, and phloretin aglycones. Total flavonoid contents of leaves (8,356.5 mg/100 g dry weight (DW)) was approximately 900-fold higher than that of fruit (fresh fruit, 13.6 mg/100 g dry DW; sun-dried fruits, 9.2 mg/100 g dry DW). Quercetin 3-O-rutinoside (rutin) and quercetin 3-O-robinobioside were the predominant flavonols in fruit and leaves of jujube. In particular, rutin had the highest content (6,735.2 mg/100 g DW) in leaves, and rutin is a widely reported bioactive compound. Phloretin 3',5'-di-C-glucoside (chalcone type) was detected only in leaves. The leaves of jujube contain a high content of flavonoids and the results of this study indicate that jujube leaves may be a source of bioactive flavonoids.

• International Journal of Industrial Entomology and Biomaterials
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• v.41 no.2
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• pp.45-50
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• 2020

Morus alba has white and/or purple fruits with a very sweet taste and low acidity. Most Korean mulberry trees have purple fruits. However, Baekokwang is a unique mulberry genetic resource in Korea with white fruits. In this study, flavonoids contents of Baekokwang mulberry leaf and fruit were analyzed using ultrahigh performance liquid chromatography coupled with diode array detection and quadrupole time-of-flight mass spectrometry (UPLC-DAD-QTOF/MS) technique. UPLC-DAD-QTOF/MS chromatogram showed that 15 flavonoids and 9 flavonoids were isolated and identified from the mulberry leaf and fruit. Total flavonoids contents of Baekokwang leaves and fruits were 812.7 mg and 35.0 mg, respectively. Baekokwang leaves had 4 major flavonoids including quercetin 3-O-(6"-O-malonyl) glucoside, 235.3 ppm, kaempferol 3-O-(6"-O-malonyl) glucoside, 132.3 ppm, kaempferol 3-O-rutinoside (nicotiflorin), 108.1 ppm, and quercetin 3-O-rutinoside (rutin), 103.8 ppm. Baekokwang fruits had 3 major flavonoids including quercetin 3-O-(6"-O-malonyl) glucoside, 13.0 ppm, quercetin 3-O-rutinoside (rutin), 7.8 ppm, and kaempferol 3-O-rutinoside (nicotiflorin), 5.7 ppm. From the above results, mulberry leaves have rich flavonoids compared to its fruits.

• Korean Journal of Pharmacognosy
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• v.47 no.2
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• pp.186-191
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• 2016

A new UPLC-DAD method for simultaneous determination of p-coumaric acid and trans-cinnamic acid in propolis was developed using Halo-C18 column and step gradient elution of MeCN and $0.1%H_3PO_4$ in 8 min. The method was validated by specificity, linearity, limit of detection, limit of quantification, precision(intra- and inter-day variability) and recovery tests. The validated method was sufficiently applicable for quantitative analysis of propolis products as well as propolis collected from different regions in Korea. The established method is simple, appropriate and efficient, and can be used for quality assessment of Korean propolis.