• 한국약용작물학회:학술대회논문집
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• 한국약용작물학회 2008년도 추계학술발표회
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• pp.477-478
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• 2008

• International Journal of Industrial Entomology and Biomaterials
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• 제37권2호
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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.

• 한국식품위생안전성학회지
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• 제32권3호
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• pp.217-221
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• 2017

Ptaquiloside는 고사리에 들어 있는 발암성 물질이다. 본 연구는 다양한 조리법에 따라 고사리에 함유된 ptaquiloside을 측정해 보고자 하였다. 조리법은 가열, 물에 침지, 물교환 횟수 등이었다. 알칼리 가수분해와 용매분획은 ptaquiloside를 화학적으로 안정한 물질인 pterosin B로 전환시켜 주었다. Pterosin B 함량은 이동상용매로 3 mM ammonium과 메탄올 용매를 사용하여 UPLC-MS/MS로 분석하였다. 조리과정이 없는 생고사리의 $H_2O$추출물에 함유된 pterosin B함량은 81 mg/kg으로 검출되어 독성물질 ptaquiloside는 46.4 mg/kg이었다. 5분의 가열 시간 후 고사리의 pterosin B 함량은 약 60%정도 제거시켜주며, 이 중 2/3는 ptaquiloside에서 전환된 pterosin B가 아닌 고사리 고유의 ptersoin B 함량이었다. 12시간 침지를 추가한 고사리는 처리하지 않은 고사리에 비해 약 88%, 또한 매시간 물교환 작업을 추가시 99.5%까지 제거됨을 알 수 있었다. 따라서 독성물질 ptaquiloside의 제거는 가열시간과 더불어 침지와 물 교환 횟수도 동시에 이루어져야 함을 알 수 있었다.

• 한국약용작물학회:학술대회논문집
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• 한국약용작물학회 2011년도 추계학술발표회
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• pp.90-91
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• 2011

• 생약학회지
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• 제47권4호
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• pp.381-388
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• 2016

Hyangso-san is a traditional herbal medicine that consists of the seven herbal medicines, Cyperi Rhizoma, Perillae Folium, Atractylodis Rhizoma, Citri Unshius Pericarpium, Glycyrrhizae Radix et Rhizoma, Zingiberis Rhizoma Crudus, and Allii Fistulosi Bulbus. Hyangso-san has long been clinically used to treat the influenza, including headache, ferver, chills, and pantalgia. In this study, we were performed the simultaneous analysis of the 15 marker compounds (liquiritin apioside, liquiritin, ferulic acid, naringin, hesperidin, rosmarinic acid, liquiritigenin, kaempferol, glycyrrhizin, nobiletin, 6-gingerol, elemicin, atractylenolide III, nootkatone, and atractylenolide I) in Hyangso-san using liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS/MS). Column for the separation of the 15 ingredients was used a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) at $45^{\circ}C$ by using a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile with gradient condition. Identifications of all analytes were performed using a Waters ACQUITY TQD LC-MS/MS system. The flow rate and injection volume were 0.3 mL/min and $2.0{\mu}L$, respectively. Correlation coefficient of the calibration curve was ${\geq}0.9958$. The values of limits of detection and quantification of the 15 components were 0.002-4.29 and 0.01-12.88 ng/mL, respectively. The result of an analysis using the established LC-MS/MS method, kaempferol and atractylenolide I were not detected, while other 13 compounds were 0.08-56.87 mg/g in lyophilized Hyangso-san sample.

• Natural Product Sciences
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• 제22권2호
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• pp.93-101
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• 2016

For efficient quality control of the Samryeongbaekchul-san decoction, a powerful and accurate an ultra-performance liquid chromatography (UPLC) coupled with electrospray ionization (ESI) tandem mass spectrometry (MS) method was developed for quantitative analysis of the thirteen constituents: allantoin (1), spinosin (2), liquiritin (3), ginsenoside Rg1 (4), liquiritigenin (5), platycodin D2 (6), platycodin D (7), ginsenoside Rb1 (8), glycyrrhizin (9), 6-gingerol (10), atractylenolide III (11), atractylenolide II (12), and atractylenolide I (13). Separation of the compounds 1 - 13 was performed on a UPLC BEH $C_{18}$ column ($2.1{\times}100mm$, $1.7{\mu}m$) at a column temperature of $40^{\circ}C$ with a gradient solvent system of 0.1% (v/v) formic acid aqueous-acetonitrile. The flow rate and injection volume were 0.3 mL/min and $2.0{\mu}L$. Calibration curves of all compounds were showed good linearity with values of the correlation coefficient ${\geq}0.9920$ within the test ranges. The values of limits of detection and quantification for all analytes were 0.04 - 4.53 ng/mL and 0.13 - 13.60 ng/mL. The result of an experiment, compounds 2, 6, 12, and 13 were not detected while compounds 1, 3 - 5, and 7 - 11 were detected with 1,570.42, 5,239.85, 299.35, 318.88, 562.27, 340.87, 12,253.69, 73.80, and $115.01{\mu}g/g$, respectively.

• 생약학회지
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• 제45권2호
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• pp.113-120
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• 2014

Generally, Gwakhyangjeonggi-san has been used for treatment of diarrhea-predominant irritable bowel syndrome. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometer method was established for the simultaneous quantification of marker compounds 1-20 in Gwakhyangjeonggi-san water extract. All analytes were separated by gradient elution using two mobile phases on a UPLC BEH $C_{18}$ ($100{\times}2.1mm$, $1.7{\mu}m$) column and maintained at $45^{\circ}C$. The injection volume was $2.0{\mu}L$ and the flow rate was 0.3 mL/min with detection at mass spectrometer. Regression equations of the compounds 1-20 were acquired with $r^2$ values ${\geq}0.9950$. The values of limit of detection and quantification of all analytes were 0.01-2.79 ng/mL and 0.03-8.37 ng/mL, respectively. The amounts of the compounds 1-20 in Gwakhyangjeonggi-san water extract were not detected $-3,236.67{\mu}g/g$. The established LC-MS/MS methods will be valuable to improve quality control of traditional herbal formula, Gwakhyangjeonggi-san.

• Journal of Ginseng Research
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• 제40권3호
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• pp.220-228
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• 2016

Background: Among the various ginseng strains, Shizhu ginseng is endemic to China, mainly distributed in Kuandian Manchu Autonomous County (Liaoning Province, China); however, not much is known about the compounds (especially saponins) in Shizhu ginseng. Methods: A rapid, sensitive, and reliable ultra-high performance liquid chromatography coupled with MS/MS (UHPLC-MS/MS) method was developed to separate and identify saponins in Shizhu ginseng. Results: The separation was carried out on a Waters ACQUITY UPLC BEH $C_{18}$ column ($100mm{\times}2.1mm$, $1.7{\mu}m$) with acetonitrile and 0.1% formic acid aqueous solution as the mobile phase under a gradient elution at $40^{\circ}C$. The detection was performed on a Micromass Quattro Micro API mass spectrometer equipped with electrospray ionization source in both positive and negative modes. Under the optimized conditions, a total of 31 saponins were identified or tentatively characterized by comparing retention time and MS data with related literatures and reference substances. Conclusion: The developed UHPLC-MS/MS method was suitable for identifying and characterizing the chemical constituents in Shizhu ginseng, which provided a helpful chemical basis for further research on Shizhu ginseng.

• 한국식품저장유통학회지
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• 제23권7호
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• pp.1004-1011
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• 2016

본 연구에서는 국내산 대추나무의 잎과 열매의 flavonoid 배당체를 조사하기 위하여 선행 연구된 인용문헌을 바탕으로 대추나무, 묏대추나무, 야생대추나무 등 대추나무속(Zizyphus)에 따른 flavonoid의 화학적 정보 수집 및 정리하여 대추나무속의 flavonoid 라이브러리를 제작하였다. 각 flavonoid 개별성분은 UPLC-DAD-QTOF-ESI/MS를 사용하여 분석하였으며 제작된 라이브러리의 정보를 이용하여 국내산 대추나무로부터 총 6종의 flavonoid를 확인하였다. 이를 통하여 국내산 대추나무 잎의 주요 성분은 quercetin 배당체인 rutin임을 확인하였고, 특히 quercetin 3-O-robinobioside 및 isoquercitrin는 구축된 라이브러리를 바탕으로 대추나무 잎에서는 처음 확인된 것을 알 수 있었다. 본 연구와 같이 대추나무속 flavonoid의 화합물 정보를 포함하여 제작한 라이브러리는 선행된 연구와의 차이점 판단을 가능하게 할 것으로 사료된다.

• 분석과학
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• 제32권1호
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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.