• 제목/요약/키워드: ultra performance liquid chromatography

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Quantitative Analysis and Enantiomeric Separation of Ephedra Alkaloids in Ma Huang Related Products by HPLC-DAD and UPLC-MS/MS

  • Kyoung-Moon Han;Jinwoo Hwang;Sun Hee Lee;Boreum Park;Hyungil Kim;Sun Young Baek
    • Natural Product Sciences
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    • 제28권4호
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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.

LC-MS/MS를 이용한 해수 및 수산용수 중 플루오로퀴놀론계 항생제 동시 분석법 정립 (Simultaneous Analysis of Prohibited Antibiotics (Fluoroquinolones) in Seawater and Effluents Released by Aquaculture Using LC-MS/MS)

  • 이미경;이인석;최민규;이성규;이원찬
    • 한국수산과학회지
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    • 제56권4호
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    • pp.428-437
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    • 2023
  • A simultaneous analytical method was developed and validated for the analysis of prohibited fluoroquinolone (FQ) antibiotics including norfloxacin, ofloxacin, and pefloxacin, released by aquaculture in seawater and effluents. The samples were filtered, and extracts were obtained using a solid phase extraction cartridge with methanol (MeOH). The extracts were concentrated, and analyzed using ultra-performance liquid chromatography-tandem mass spectrometry. Two different columns and four different mobile phases were compared to achieve optimal separation and sensitivity for target compounds. Typical validation parameters including linearity, recovery of surrogate standard, instrument detection limit (IDL), limit of quantification (LOQ), and method detection limit (MDL) were evaluated. The linearity of calibration curves was over 0.999. Recoveries of surrogate ranged from 87.6% to 113%. The LOQ of target compounds was approximately 3-8 times lower than those reported in previous studies. The IDL and MDL were 0.06-0.57 and 0.06-0.37 ng/L, respectively. Seven effluent samples collected from an aquaculture located in Jeju were analyzed; however, not all target compounds were detected in the samples, suggesting that the banned antibiotics were not used. Overall, this established method was able to simultaneously analyze the three FQ antibiotics, and may be useful for monitoring prohibited antibiotics in the fishery industry.

Occupational Exposure during Intraperitoneal Pressurized Aerosol Chemotherapy Using Doxorubicin in a Pig Model

  • Wongeon Jung;Mijin Park;Soo Jin Park;Eun Ji Lee;Hee Seung Kim;Sun Ho Chung;Chungsik Yoon
    • Safety and Health at Work
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    • 제14권2호
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    • pp.237-242
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    • 2023
  • Background: This study evaluated occupational exposure levels of doxorubicin in healthcare workers performing rotational intraperitoneal pressurized aerosol chemotherapy (PIPAC) procedures. Methods: All samples were collected during PIPAC procedures applying doxorubicin to an experimental animal model (pigs). All procedures were applied to seven pigs, each for approximately 44 min. Surface samples (n = 51) were obtained from substances contaminating the PIPAC devices, surrounding objects, and protective equipment. Airborne samples were also collected around the operating table (n = 39). All samples were analyzed using ultra-high performance liquid chromatography-mass spectrometry. Results: Among the surface samples, doxorubicin was detected in only five samples (9.8%) that were directly exposed to antineoplastic drug aerosols in the abdominal cavity originating from PIPAC devices. The telescopes showed concentrations of 0.48-5.44 ng/cm2 and the trocar showed 0.98 ng/cm2 in the region where the spraying nozzles were inserted. The syringe line connector showed a maximum concentration of 181.07 ng/cm2, following a leakage. Contamination was not detected on the surgeons' gloves or shoes. Objects surrounding the operating table, including tables, operating lights, entrance doors, and trocar holders, were found to be uncontaminated. All air samples collected at locations where healthcare workers performed procedures were found to be uncontaminated. Conclusions: Most air and surface samples were uncontaminated or showed very low doxorubicin concentrations during PIPAC procedures. However, there remains a potential for leakage, in which case dermal exposure may occur. Safety protocols related to leakage accidents, selection of appropriate protective equipment, and the use of disposable devices are necessary to prevent occupational exposure.

Impact of Korean Malting Barley Varieties on Malt Quality

  • Young-Mi Yoon;Jin-Cheon Park;JaeBuhm Chun;Yang-Kil Kim;Hyeun-Cheol Cheo;Chang-Hyun Lee;Seul-Gi Park;Tae-Il Park
    • 한국작물학회:학술대회논문집
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    • 한국작물학회 2022년도 추계학술대회
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    • pp.18-18
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    • 2022
  • Barley has been used for the production of malt in the brewing industry. Malting is the process of preparing barley through partial germination. Malt extract is the most important quality parameter for malt quality. The grain and malt quality parameters of ten Korean malting barley varieties were studied. Malts was prepared using Phoeix automated micro malting system(Phoenix Bio, Australia). Quality analysis of Barley and malt was determined according to European brewery convention(EBC, 1998) and American society of brewing chemists(ASBC, 1997) method. And the hordeins of barley and malt were extracted with 50% isopropyl alcohol(IPA, 2-propanol) of 1% dithiothreitol(DTT). The analysis of hordeins was carried out by ultra-performance liquid chromatography(UPLC). The mean values of 1000-grains weight, assortment rate, protein content, starch content, beta-glucan content, husk rate, germination energy, germination capacity and water sensitivity of grain were 45.8g, 86.8%, 11.9%, 58.0%, 3.8%, 14.0%, 96.2%, 97.2%, 10.0%, respectively. The mean values of protein content, friability, diastatic power, extract, soluble protein, Kolbach index, beta-glucan of malt and wort were 11.3%, 87.6%, 201WK(Windish Kolbach), 79.3%, 4.6%, 41%, 85mg/L, respectively. UPLC analysis of grain and malt hordeins revealed that the amount of hordeins significantly degraded during malting. Also, we could successfully be used to compare hordein polypeptide patterns with malt quality.

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Effect of Plant Growth Regulator Treatment on Isoflavones in Soybean

  • Jinhee Seo;Seoyeon Hong;Hyerang Park;Jaesung Park;Okjae Won;Eunji Seo;Wonyoung Han;Kido Park
    • 한국작물학회:학술대회논문집
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    • 한국작물학회 2022년도 추계학술대회
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    • pp.164-164
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    • 2022
  • The soybean (Glycine max(L.) Merrill), an important food crop in the world, is popular because of its high quality protein and oil content. Soybeans as a food have long been known for their beneficial effects on health and are well-recognized globally. Isoflavones, significant soybean secondary metabolic products, may be crucial in avoiding some cancers and lowering the risk of cardiovascular disorders. This study investigates the correlation between plant growth regulator and the effect on the isoflavone levels in soybean leaves. The study was carried out in the green-house of the southern crop department in miryang. Soybeans(Seonpung) were cultivated in 1/2000 of the Wagner pot. Ethephon(500, 1000, 2000 ppm) and ABA(100, 200, 400 ppm) were used as plant growth regulators, and they were each treated on R2, R5, and R7 stage. After treatment, leaves were sampled three times at intervals of 5 days, and the content of 6 isoflavones and coumestrol was analyzed. Soybean isoflavones were analyzed using Ultra Performance Liquid Chromatography (Acquity UPLC H-Class system, Waters). The isoflavones content showed an overall highly in the R5 stage, and the level was similar to that of no treatment in the R2 and R7 stage. The difference between the growth regulators was found to be higher than that of ethephon when ABA was treated. The coumestrol content was confirmed to be high in the order of R7, R5, and R2 on the treatment time, and it was found that the content increased as the treatment time was delayed. In the treatment with the growth regulator, the coumestrol content tended to be higher when ethephon was treated than ABA.

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Selection of Resistant Varieties to Aspergillus flavus by Determination of Aflatoxin B1 Content in Korean Peanut (Arachis hypogaea L.) Accessions

  • Seungah Han;Byeong-Cheol Kim;Jungmin Ha;Tae-Hwan Jun
    • 한국작물학회지
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    • 제68권3호
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    • pp.175-187
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    • 2023
  • Peanuts, also known as groundnuts (Arachis hypogaea L.), are globally recognized as a vital oilseed crop. Peanuts are rich in proteins (e.g., arginine), oils (e.g., oleic acid and linoleic acid), fiber, vitamins (e.g., niacin and tocopherol), and carbohydrates and are consumed worldwide. However, the presence of aflatoxin (AF) has garnered substantial attention since its initial discovery as the causative agent of Tukey's X disease in the United Kingdom in 1960. Among the 18 aflatoxins identified, aflatoxin B1 (AFB1) has the highest toxic activity and causes hepatocellular carcinoma. It is classified as Group I by the International Agency for Research on Cancer (IARC) of the World Health Organization (WHO). The present study was conducted to evaluate aflatoxin B1 resistance of 102 peanut accessions and select putative aflatoxin B1-resistant peanut accessions to aflatoxin B1. One hundred and one Korean germplasms harvested in 2020 were inoculated with A. flavus to identify aflatoxin-resistant cultivars, and the aflatoxin B1 concentration was measured using an ultra-performance liquid chromatography-photodiode array detector. Twenty-six accessions with aflatoxin B1 concentrations lower than those of the check plant 55-437 were chosen for the development of aflatoxin-resistant varieties in Korea. As Korean aflatoxin-resistant varieties have not yet been developed, the findings of the present study are expected to provide useful information for the development of aflatoxin-resistant cultivars.

한국산 오디 품종별 안토시아닌 배당체 성분 분석 (Analysis of Anthocyanin Glycosides in Korean Mulberry Fruit Cultivars)

  • 김소아;권령하;김주형;라혜민;이지혜;조수묵;김헌웅
    • 한국식품영양학회지
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    • 제36권6호
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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.

갯까치수염(Lysimachia mauritiana Lam.)의 재배 및 UHPLC 패턴 분석, 호흡기염증 억제 효과 (Cultivation, UHPLC Pattern Analysis, and Inhibitory Effect on Respiratory Inflammation of Lysimachia mauritiana Lam.)

  • 김동선;육흥주;김정미;고채석;장윤정;성윤영
    • 대한본초학회지
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    • 제39권3호
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    • pp.77-84
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    • 2024
  • Objectives : Lysimachia mauritiana Lam. is known as a medicinal plant native to Korea that has antioxidant, anticancer, antibacterial, and antiviral activities. However, until now, research on the cultivation technology of L. mauritiana is insufficient, and there are no research data on the systematic cultivation method and mass production of L. mauritiana. Therefore, this study aims to establish a cultivation system of L. mauritiana. Methods : The cultivation environment of open land and facilities according to the growth of L. mauritiana was compared and tested. In addition, the equivalence of the origin collection extract and the cultivation extract was evaluated through Ultra high performance liquid chromatography (UHPLC) patterns analysis according to cultivation and comparison of the effect of inhibiting respiratory inflammation using BEAS-2B human bronchial epithelial cells. Results : The cultivation technology system was established through cultivation research of L. mauritiana raw materials. In addition, as a result of comparing and evaluating the equivalence of cultivated plants and L. mauritiana raw materials for suppressing respiratory inflammation, the same results were confirmed, and the equivalence was confirmed as a result of analyzing the UHPLC pattern with L. mauritiana raw materials. Conclusions : This study suggests that extract from cultivation research of L. mauritiana plants, which are native to Korea, can be used as a health functional food or medicine to improve respiratory health.

Methiozolin의 분석법 개발 및 골프장 그린에서의 잔류소실특성 (Establishment of analytical method of methiozolin and dissipation in golf course's green)

  • 조형욱;황규원;황기환;문준관
    • Journal of Applied Biological Chemistry
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    • 제59권4호
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    • pp.331-336
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    • 2016
  • Methiozolin의 토양, 유출수, 잔디 중 잔류 분석법 확립 및 토양과 그린잔디에서 잔류량 감소현상을 연구하였다. 잔류량은 acetone으로 추출 후, dichloromethane으로 분배하고, SPE를 이용하여 정제하여 자외선 검출기가 부착된 HPLC로 280 nm에서 검출하였다. 최소검출량과 정량한계는 유출수, 잔디, 토양에서 각각 1.0, 0.5, 1.0 ng과 0.001, 0.1, 0.01 mg/kg이었다. 분석법의 회수율은 유출수, 잔디, 토양에서 각각 87.5~111.3, 92.8~97.4, 78.2~98.5 %로 methiozolin 잔류분석에 적합하였다. 골프 코스 그린에 약제 처리 후 0, 1, 4, 7, 14, 30, 45, 60일차에 토양과 잔디시료를 채취하여 분석한 결과, methiozolin 잔류량은 하부 토양으로 이동현상이 관찰되지 않았고, 잔디와 잔디 근권토양에 존재하였다. 잔디와 토양 중 반감기는 각각 10.7일과 8.8일로 확인되었다.

UHPLC를 이용한 볏짚 사일리지와 동계사료작물의 오크라톡신과 제랄레논 분석법 최적화 (Optimization of Analytical Methods for Ochratoxin A and Zearalenone by UHPLC in Rice Straw Silage and Winter Forage Crops)

  • 함현희;문혜연;이경아;이수형;홍성기;이데레사;류재기
    • 한국초지조사료학회지
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    • 제36권4호
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    • pp.333-339
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    • 2016
  • 조사료에서 오크라톡신 A (OTA) 및 제랄레논(ZEA)의 단성분 분석법을 최적화하기 위하여 곰팡이 독소에 오염되지 않은 볏짚 사일리지, 이탈리안 라이그라스, 청보리, 호밀을 대상으로 각 시료 별로 OTA는 50, 250, $5,000{\mu}g/kg$, ZEA는 300, 1,500, $3,000{\mu}g/kg$의 농도로 스파이킹하고 면역친화성 컬럼을 이용하여 독소를 정제한 후 UHPLC-FLD를 이용하여 분석하였다. 분석 결과 표준용액의 검량선은 OTA가 결정계수 0.9999, ZEA가 0.9995로 높은 직선성을 나타냈으며, 검출 및 정량한계는 OTA가 각각 $0.1{\mu}g/kg$, $0.3{\mu}g/kg$, ZEA는 각각 $5{\mu}g/kg$, $16.7{\mu}g/kg$을 나타냈다. 유효성 및 정밀성 검정결과 OTA는 볏짚이 회수율 84.23~95.33%, 상대표준편차 (RSD) 2.59~4.77%, 이탈리안 라이그라스는 회수율 79.02~95%, RSD 0.86~5.83%, 청보리는 회수율 74.93~97%, RSD 0.85~9.19%, 호밀은 회수율 77.99~96.67%, RSD 0.33~6.26%를 나타냈으며, ZEA는 볏짚이 회수율 109.6~114.22%, RSD 0.67~7.15%, 이탈리안 라이그라스는 회수율 98.01~109.44%, RSD 1.65~4.81%, 청보리는 회수율 98~113.53%, RSD 0.25~5.85%, 호밀은 회수율 90.44~108.56%, RSD 2.5~4.66%를 나타내어 유럽연합에서 제시한 기준을 만족하였다. 따라서 본 연구에서 제시한 분석법은 국내의 볏짚 등 조사료 4종에서 OTA와 ZEA의 분석에 활용할 수 있음을 시사하였다.