• Title/Summary/Keyword: UPLC method

검색결과 107건 처리시간 0.022초

경기도내 유통 수입과실류의 잔류농약 실태조사 (A survey on pesticide residues of imported fruits circulated in Gyeonggido)

  • 조윤식;강정복;김양희;정진아;허정원;이소현;임영식;배호정;강흥규;이정희;정은숙;이병훈;박용복;이정복
    • 농약과학회지
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    • 제16권3호
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    • pp.195-201
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    • 2012
  • 본 연구는 경기도에서 유통 중인 수입과실류에 대한 잔류농약 분석을 수행하였다. 총 22품목 124건의 시료를 구입하여 GC/NPD-ECD, TOF/MS, UPLC/PDA 및 HPLC/FLD, LC/MS/MS를 이용하여 218종 잔류농약을 동시 다성분 분석법으로 분석한 결과 18건의 과실에서 잔류농약이 0.003~0.3 mg/kg 범위로 검출되었으나 기준초과 시료는 없었다. 과실의 부위별 특성에 따른 잔류농약정도를 알아보기 위해 농약이 검출된 과실류 중 14건에 대하여 분리 실험을 실시하였으며, 그 결과 과피 14건에서 0.03~1.5 mg/kg, 과육의 경우 2건에서 검출한계 미만으로 나타났다. 실험결과 모두 잔류농약허용기준 이내에서 검출되어 정상적인 방법으로 섭취할 경우 위해도는 매우 낮은 수준이었다. 그러나 미량이라도 장기간 섭취시 인체에 유해할 수 있으며, 검출빈도가 높은 성분들이 검출되므로 수입과실에 대한 지속적이고 체계적인 모니터링이 필요하겠다.

구강질환 세균에 대한 한약재의 항균효과 (Antibacterial Effect of Oriental Medicinal Herbs on Dental Pathogens)

  • 유영은;박은영;정대화;변성희;김상찬;박성민
    • 미생물학회지
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    • 제46권2호
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    • pp.200-206
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    • 2010
  • 본 연구에서는 69가지의 한약재를 이용하여 구강세균인 Actinomyces viscocus, Streptococcus sobrinus, 그리고 Streptococcus mutans 2종에 대한 항균효과를 조사하였다. 우선 선발된 한약재를 메탄올로 추출하여 조사하였으며 그 결과를 바탕으로 소목, 오매, 오미자, 그리고 황련을 선별하여 열수, 에탄올, 메탄올, 그리고 에틸아세테이트를 이용하여 항균효과를 조사하였다. 조사결과 황련 열수 추출물이 가장 우수한 효과를 나타내는 것으로 조사되었다. 황련 열수 추출물을 이용하여 공시균주에 대한 저해양상을 조사한 결과 180 mg/ml 이상의 농도에서 공시균주의 생육이 대부분 저해되는 것을 확인할 수 있었으며 이 때 황련 열수 추출물의 회수율은 22%였다. 황련 열수 추출물을 UPLC를 이용하여 berberine 함량을 조사한 결과 25.54%로 조사되었다. 또한 $121^{\circ}C$에서 15분간 열 처리 후 황련 열수 추출물의 열 안정성을 조사한 결과 열에 대하여 안정 하다는 것을 확인할 수 있었다.

β-카볼린 화합물의 합성 및 구조분석 (Synthesis and Structural Characterization of β-Carboline Compounds)

  • 변홍주;한민희;문기성;정경환;이향렬
    • 한국응용과학기술학회지
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    • 제36권2호
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    • pp.676-684
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    • 2019
  • 자연에서도 생합성이 되는 테트라하이드로-${\beta}$-카볼린 화합물은 Pictet-Spengler반응을 통해서 화학적으로도 합성된다. 본 연구에서는 ${\beta}$-카볼린 화합물을 쉽고 효과적으로 합성할 수 있는 친환경 합성법을 개발하여 유기용매가 아닌 물을 사용하여 합성하였다. 이 화합물은 투명한 결정형의 생성물로 얻어지므로 복잡한 분리과정이 필요하지 않다. 합성된 화합물은 NMR 및 UPLC/MS를 이용하여 구조를 확인하였다. 화합물 1의 이론적 분자량($C_{17}H_{17}N_2$ 249.1392), 화합물 2 ($C_{17}H_{23}N_2$ 255.1861), 화합물 3($C_{19}H_{21}N_2O_3$ 325.1552), 화합물 4($C_{19}H_{19}N_2O$ 279.1497)과 측정된 화합물들의 질량과 비교하였다. 그 결과 측정된 화합물 1의 분자량 ($[M+H]^+m/z$ detected 249.1315), 2 (detected 255.1789), 3 (detected 325.1460) 그리고 4 (detected 279.1364)와 거의 일치함으로써 생성된 화합물이 1~4의 구조를 가지고 있음을 확인하였다. 합성된 화합물들을 그람 음성균인 E. coli $DH5{\alpha}$를 대상으로 항균효과를 조사한 결과 강한 저해효과를 확인할 수 있었다.

잡곡 농산물의 잔류농약 안전성 조사 (A Study on the Safety of Residual Pesticides in Cereal Grains and Pulses Agricultural Products Excluding Rice)

  • 한나은;김재관;윤희정;강민성;조영선;송지원;김병태;이성남;최옥경
    • 한국식품위생안전성학회지
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    • 제37권1호
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    • pp.1-8
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    • 2022
  • 본 연구는 2021년 2월부터 7월까지 잡곡 106건을 수거하여 잔류농약 실태조사를 하였다. 대형, 중소형 및 온라인 유통매장을 중심으로 국내 잡곡 40건과 수입 잡곡 66건을 수거하였고, GC/MSMS, GC/ECD, GC/NPD, LC/MSMS, UPLC/PDA, HPLC/FLD를 이용하여 다종농약 다성분분석법으로 잔류농약 341종을 분석하였다. 잔류농약이 검출된 잡곡은 대형유통매장 1건, 중소형 유통매장 2건, 온라인 유통매장 5건으로 총 8건(7.5%)이었고, 5건(4.7%)에서는 농약잔류허용기준을 초과하였다. 이들 잡곡에서는 MGK-264, chlorpyrifos, thiamethoxam, malathion, piperonyl butoxide, pirimiphos-methyl 등 6종의 농약 성분이 검출되었다. 검출된 잡곡은 강낭콩(1건), 녹두(6건), 수수(1건)이다. 검출된 잡곡 중 농약잔류허용기준을 초과한 품목은 수입 녹두(5건)로 미얀마산이었고, 초과한 농약 성분은 thiamethoxam이었다.

LC-MS/MS를 이용한 곽향정기산(藿香正氣散) 추출물 중 20종 성분의 함량분석 (Quantitative Analysis of the Twenty Marker Components in Gwakhyangjeonggi-san using Ultra-Performance Liquid Chromatography with Mass Spectrometer)

  • 서창섭;신현규
    • 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.

인동(忍冬)의 기철(忌鐵) 및 반철(伴鐵) 추출시(抽出時) 추출물(抽出物)의 변화(變化) (Extract changes of Caulis Lonicerae Japonicae according to with or without Iron)

  • 정덕자;정대화;장미희;박정아;김상찬
    • 대한한의학방제학회지
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    • 제28권3호
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    • pp.281-287
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    • 2020
  • Objectives : In case of herbs decoction, the ceramic or earthware pots was recommended, but not the metals, particularly iron or aluminum, which could cause unknown chemical reactions. In Korean Medical classics, it has been known that some herbs including Caulis Lonicerae Japonicae (CL) were not recommended to boil with iron pot. This study investigates the physical changes of extracts of CL with or without iron. Methods : CL was decocted with reflux cooling extraction system to prevent evaporation and volatilization. Content of polyphenol was detected by Folin-Denis method and the levels of loganin and chlorogenic acid were evaluated by UPLC. Results : The color of extract with glass beads (GB) is yellowish brown, and the iron beads (IB) is blackish brown. Polyphenol and chlorogenic acid levels were reduced in IB extracts. Conclusions : The color of extract was change to blackish brown, and polyphenol and chlorogenic acid levels were reduced in CL extract with iron. Therefore, iron pots is not suitable for CL extraction.

구강미생물에 대한 고삼의 항균효과 (Antimicrobial Effects of Sophorae Radix Extracts against Oral Microorganisms)

  • 박숙자;김상찬;이종록
    • 대한본초학회지
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    • 제25권2호
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    • pp.81-88
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    • 2010
  • Objectives : Sophorae Radix (SR), the dried root of Sophorae Flavescens Aiton, has been used to treat atherosclerosis, arrhythma and skin diseases including scabies and eczema. The present study was examined to evaluate antimicrobial activities of SR extracts against oral microorganism. Methods : Antimicrobial properties of SR extracts were determined by agar diffusion method and minimum inhibitory concentration (MIC) against Streptococcus mutans, Streptococcus sobrinus and Actinomyces viscosus. Analysis of kurarinone from SR extracts was conducted using UPLC (Ultra Performance Liquid Chromatography). Results : The ethanolic extracts of SR showed stronger antimicrobial effect than methanolic extracts, while the aqueous extracts of SR had no activity. In addition, the higher content of kurarinone was found in ethanolic extracts than methanolic extracts. The purified kurarinone from ethanolic extracts showed potent antimicrobial activity with the MIC value of $3.9{\sim}7.8{\mu}g/m{\ell}$. Conclusion : An ethanolic extract of SR showed antimicrobial properties against several oral microorganisms, and kuranrinone contributed to antimicrobial action of SR. Thus, ethanolic extracts of SR or purified kurarinone should be beneficial for the preparation of the useful agent for treating oral disease including anticaries.

단백체 분석을 위한 일차원 및 이차원 역상크로마토그래피의 비교 (Comparison of 2-D RP-RP MS/MS with 1-D RP MS/MS for Proteomic Analysis)

  • 문평곤;조영은;백문창
    • 약학회지
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    • 제54권5호
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    • pp.377-386
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    • 2010
  • Single-dimensional (1-D) and two-dimensional (2-D) LC methods were utilized to separate peptides from various sources followed by MS/MS analysis. Two-dimensional ultra-high performance liquid chromatography is a useful tool for proteome analysis, providing a greater peak capacity than 1-D LC. The most popular 2-D LC approach used today for proteomic research combines strong cation exchange and reversed-phase LC. We have evaluated an alternative mode for 2-D LC of peptides using 2-D RP-RP nano UPLC Q-TOF Mass Spectrometry, employing reversed-phase columns in both separation dimensions. As control experiments, we identified 129 proteins in 1-D LC and 322 proteins in 2-D LC from E. coli extract peptides. Furthermore, we applied this method to rat primary hepatocyte and a total of 170 proteins were identified from 1-D LC, and 527 proteins were identified from all 2-D LC system. The in-depth protein profiling established by this 2-D LC MS/MS from rat primary hepatocyte could be a very useful reference for future applications in regards to drug induced liver toxicity.

Structural Identification of Modified Amino Acids on the Interface between EPO and Its Receptor from EPO BRP, Human Recombinant Erythropoietin by LC/MS Analysis

  • Song, Kwang-Eun;Byeon, Jaehee;Moon, Dae-Bong;Kim, Hyong-Ha;Choi, Yoo-Joo;Suh, Jung-Keun
    • Molecules and Cells
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    • 제37권11호
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    • pp.819-826
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    • 2014
  • Protein modifications of recombinant pharmaceuticals have been observed both in vitro and in vivo. These modifications may result in lower efficacy, as well as bioavailability changes and antigenicity among the protein pharmaceuticals. Therefore, the contents of modification should be monitored for the quality and efficacy of protein pharmaceuticals. The interface of EPO and its receptor was visualized, and potential amino acids interacting on the interface were also listed. Two different types of modifications on the interface were identified in the preparation of rHu-EPO BRP. A UPLC/Q-TOF MS method was used to evaluate the modification at those variants. The modification of the oxidized variant was localized on the Met54 and the deamidated variants were localized on the Asn47 and Asn147. The extent of oxidation at Met54 was 3.0% and those of deamidation at Asn47 and Asn147 were 2.9% and 4.8%, respectively.

LC-MS/MS를 이용한 당귀수산 추출물 중 17종 성분의 함량분석 (Quantitative Analysis of the Seventeen Marker Components in Dangguisu-san Using Ultra-performance Liquid Chromatography Coupled to Electrospray Ionization Tandem Mass Spectrometry)

  • 서창섭;신현규
    • 약학회지
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    • 제58권3호
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    • pp.158-164
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    • 2014
  • Dangguisu-san is a well-known traditional Korean herbal medicine prescription and has been widely used to treat ecchymosis, blood stagnation, and pain resulting from physical shock in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometer method was established for the simultaneous determination of the 17 biomarker components in Dangguisu-san. All analytes were separated on an UPLC BEH $C_{18}$ ($100{\times}2.1$ mm, $1.7{\mu}m$) column and maintained at $45^{\circ}C$. The mobile phase consisted of two solvent systems, 0.1% (v/v) formic acid in water (A) and acetonitrile (B) by gradient flow. The injection volume was $2.0{\mu}l$ and the flow rate was 0.3 ml/min with detection at mass spectrometer. Calibration curves of the 17 biomarker components were acquired with $r^2$ values ${\geq}0.9951$. The values of limit of detection and quantification of all analytes were 0.02~6.32 ng/ml and 0.05~18.95 ng/ml, respectively. The amounts of the 17 components in Dangguisu-san sample were $3.17{\sim}13,224.50{\mu}g/g$.