• 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 Food Science and Technology
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• v.44 no.6
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• pp.686-691
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• 2012

The objective of this research is to present method development and validation for the simultaneous determination of lutein and zeaxanthin using ultra performance liquid chromatography (UPLC). Also, rapid quantification was performed on six green leafy vegetables (Allium tuberosum, Aster scaber, Hemerocallis fulva, Pimpinella brachycarpa, Sedum sarmentosum and Spinacia oleracea) that are commonly consumed in Korea. Separation and quantification were successfully achieved with a Waters Acquity BEH C18 ($50{\times}2.1mm$, $1.7{\mu}m$) column by 85% methanol within 5 min. Two compounds showed good linearity ($r^2$ > 0.9968) in $1-150{\mu}g/mL$. Limit of detection (LOD) and quantification (LOQ) for lutein and zeaxanthin were 1.7 and 5.1 g/mL and 2.1 and 6.3 g/mL, respectively. The RSD for intra- and inter-day precision of each compound was less than 10.69%. The recovery of each compound was in the range of 91.75-105.13%. Aster scaber and Spinacia oleracea contained significantly higher amounts of lutein ($4.06{\pm}0.24$ and $3.97{\pm}0.10mg$/100 g of fresh weight), respectively.

• Journal of the Korean Wood Science and Technology
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• v.44 no.3
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• pp.337-349
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• 2016

In this study, an analytical method to evaluate the quality of isoflavonoid compounds purified and isolated from the fruits of Cudrania tricuspidata was developed and validated using Ultra Performance Liquid Chromatography (UPLC). The fruits of C. tricuspidata were extracted with methanol and further fractioned with n-hexane, ethyl acetate and water. The resulting ethyl acetate extract separated into four isoflavonoid compounds by a combination of silica gel and sephadex LH-20 column chromatography. The structures of the compounds were elucidated as alpinumisoflavone, 6,8-diprenyl genistein, 6,8-diprenyl orobol, 4'-O-methylalpinumisoflavone by various techniques such as UV-Vis, ESI-MS, $^1H\;NMR$ and $^{13}C\;NMR$ spectroscopy. Finally, a method to characterize the compounds was developed by using the UPLC equipped with a $C_{18}$ column and a gradient mobile phase system consisting of 2% acetic acid in water (solvent A) and 2% acetic acid in methanol (solvent B). The developed method was validated with the parameters such as selectivity, linearity, limit of detection, limit of quantitation, accuracy, and precision, which are defined by the ICH (International Conference on Harmonization). Using the validated method, the compounds in the fruits harvested in different months were also quantitatively analyzed. We propose this approach this approach can readily be utilized as an efficient evaluation method to quantify the extracts of C. tricuspidata.

• 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.

• Bulletin of Food Technology
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• v.21 no.2
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• pp.49-54
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• 2008

농산물 중 잔류농약을 보다 쉽고 효율적으로 분석 할 수 있는 다성분 동시분석 방법에 따라서 UPLC-PDA을 이용하여 기기조건에 따른 검출한계 및 정량한계를 식품별 최저 MRL과 비교하여 유효성을 알아보고 회수율을 통하여 방법의 재현성을 조사한 결과 다음과 같다. 41종의 농약에 대한 검량선은 직선성이 우수하였으며 검출한계 $0.005{\sim}0.109mg/kg$으로 나타났으며 정량한계 는 $0.018{\sim}0.363ppm$으로 나타났다. Cycloprothrin 등의 경우처럼 검출기의 감응도가 최저 MRL 기준을 초과하는 농약에 대한 보완으로는 검출감도가보다 우수한 UV 검출기 등의 병행 활용이 필요하다. 회수율에 따른 재현성은 쌀의 경우 첨가 농도 0.4 mg/kg 일때 $62.09{\sim}99.58%$로 편차범위는 $1.03{\sim}13.92%$ 얻을 수 있었다.

• 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.

• Analytical Science and Technology
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• v.32 no.1
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• pp.24-34
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• 2019

The safety of food is occasionally questionable, as there have been some reports of products contaminated with illegal adulterants. In this study, the presence of 16 sedative-hypnotics and sleep inducers in dietary supplements was determined by ultra-high-performance liquid chromatography with UV detection (UPLC-UV) and quadruple Orbitrap mass spectrometry (Q-Orbitrap-MS). The UPLC method was validated, providing a linearity (R2) of more than 0.999, and LODs and LOQs that ranged from 0.2 to 0.5 and 0.6 to $1.5{\mu}g\;mL^{-1}$, respectively. The repeatabilities were 0.2-8.4 % (intra-day) and 0.3-4.5 % (inter-day), and the accuracies were 89.0-117.0 % (intra-day) and 87.8-111.9 % (inter-day). The mean recoveries of the spiked samples ranged from 98.7 to 107.3 %. The relative standard deviation (%RSD) of the stability was less than 2.4 %. Using the developed method, one sedative-hypnotic compound, phenobarbital, was detected in one of the nineteen samples tested. In addition, the major characteristic fragment ions of each target compound were confirmed using Q-Orbitrap-MS for higher accuracy. Monitoring the presence of these 16 sedative-hypnotics and sleep inducers in dietary supplements should be pursued in the interest of human health, and the results of this study confirmed that the developed method has value for this application.

• Journal of Apiculture
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• v.32 no.3
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• pp.253-259
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• 2017

Propolis, natural antibacterial agent, which has been used traditional medicine across the globe, is resinous mixture to include abundant bioactive substances. In present study, we investigated antimicrobial activity according to quality characteristics of propolis collected from 9 different regions in Korea. Antimicrobial activity was evaluated by measuring growth inhibition zone using agar well diffusion method against Streptococcus mutans. Constituents analysis of propolis samples were measured through total phenolic contents, total flavonoid contents and quantitative analysis of major compound (pinocembrin) by ultra performance liquid chromatography. As a result, 9 different propolis (10mg/mL) and pinocembrin (1mg/mL) showed antimicrobial activity that has growth inhibition zone more than 11.9mm on S. mutans. The total flavonoid contents of 8 different propolis excluding Jeju island were in compliance with standard of health functional food in Korea and were found to affect antimicrobial activity on S. mutans when contained over 10mg/g. In addition, when content of pinocembrin in propolis was ranged from 12mg/g to 32mg/g, each propolis excluding Jeju island exhibited antimicrobial activity alike. These results indicate that pinocembrin plays a important role for antimicrobial activity of propolis collected from 8 different regions in Korea, and that it can be used as basic data for standardization of Korean propolis.

• Journal of Applied Biological Chemistry
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• v.65 no.4
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• pp.343-348
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• 2022

This study was performed to establish an analytical method for the standardization of Angelicae Dahuricae Radix as a functional ingredient. We established six compounds including oxypeucedanin hydrate (1), byakangelcol (2), oxypeucedanin (3), imperatorin (4), phellopterin (5) and isoimperatorin (6) as marker compounds of Angelicae Dahuricae Radix. An analytical method using Ultra Performance Liquid Chromatography (UPLC) was established and validated for marker compounds of Angelicae Dahuricae Radix. The specificity was confirmed by the chromatogram from UPLC and the value of coefficient determination was also higher than 0.999, indicating high linearity. The relative standard deviation (RSD) and recovery of marker compounds were less than 5% and in the range of 90- 110%, respectively, which means that this method has high accuracy and precision. Therefore, this analytical method could be used as basic data for the development of functional ingredients for health functional food of Angelicae Dahuricae Radix.

• Proceedings of the Korean Society of Crop Science Conference
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• 2021.04a
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• pp.122-122
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• 2021