• 제목/요약/키워드: MS analysis

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LC/MS/MS를 이용한 석류추출물 중의 에스트로겐 분석 (Analysis of Estrogen in Pomegranate Extract by Solid Phase Extraction and Liquid Chromatography Tandem Mass Spectrometry)

  • 금은주;권도형;신혜승
    • 한국식품위생안전성학회지
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    • 제25권1호
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    • pp.79-82
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    • 2010
  • 석류는 오래전부터 임상치료 및 식품원료로 사용되었으며 많은 피토에스트로겐 성분을 함유하고 있다. 그 성분으로는 에스트론, 에스트라디올, 에스트리올, 베타-시토스테롤, 엘라그산 등이 였으며 이러한 성분으로 인해 과즙, 껍질, 오일 등은 약한 에스트로겐 활성을 나타낸다고 보고되었으며, 이로 인해 석류는 여성 갱년기 치료용 원료로 많이 사용되고 있다. 그러나 에스트로겐 성분의 존재 유무에 대한 견해의 차이가 나타나고 있어 본 연구는 LC/MS/MS를 이용하여 석류추출물 중의 에스트로겐 분석을 통해 이를 확인하고자 하였으며, 간편하고 정확한 분석법을 모색하고자 하였다. 3개 롯트 시료의 에스트로겐을 분석한 결과, 에스트론 83.5ppb, 에스트라디올 10.9ppb 및 에스트리올 38.6ppb로 검출되었다.

CDMA-2000 서비스를 위한 VoIP 기반 망에서 Mobile IP를 이용한 음성/데이타 통합 및 성능평가 (Voice/Data Integration and Performance Analysis using Mobile If on the VoIP Network for the service of CDMA-2000)

  • 엄기복;여현;이윤주
    • 한국정보통신학회:학술대회논문집
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    • 한국해양정보통신학회 2001년도 추계종합학술대회
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    • pp.89-92
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    • 2001
  • Mobile IP 망에서 보다 좋은 품질의 서비스를 제공하기 위한 하나의 방법으로 RSVP 및 WFQ를 제안하였다. 성능평가를 위하여 Mobile IP와 VoIP 네트워크 Model를 구성하였고, 지연 및 QoS에 관한 성능평가를 실시하였다. 성능평가 결과 Mobile agent 가 이동전에는 2ms, 이동후에는 3ms, QoS를 적용하기 전에는 30ms, QoS를 적용한 후에는 10ms가 분석되었다. 본 논문에서는 QoS를 적용하여 Mobile IP 망에서 지연 문제를 개선시켰다.

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제주 지역 성인의 담낭용종 유병률 및 대사증후군과의 관련성 (The association between prevalence of gallbladder polyp and metabolic syndrome in Jeju Island adults)

  • 권오성;김영규;정진영
    • 한국컴퓨터정보학회:학술대회논문집
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    • 한국컴퓨터정보학회 2020년도 제62차 하계학술대회논문집 28권2호
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    • pp.151-154
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    • 2020
  • Metabolic syndrome (MS) is increasing as obesity increases in Korea. In this study, we investigated the relationship between MS and gallbladder polyp (GBP). We examined 9,861 subjects who visited a single health-screening center in Jeju between January 2009 and December 2019. MS was defined according to the revised National Cholesterol Education Program criteria. Multiple logistic regression analysis was performed after adjusting for age to evaluate the association between the components of MS and GBP. The estimated rates of MS and GBP among subjects were 28.5% and 4.8%, respectively. Multivariate analysis suggested that MS (odds ratio[OR] 1.405, P=0.006) was the only independent factor affecting GBP. In our study sample, MS was correlated with GBP. The prevalence of gallbladder polyp increased with an increase in the risk factors indicating MS.

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LC-MS/MS를 이용한 설사성패류독소의 분석조건 확립 (Establishment of a Method for the Analysis of Diarrhetic Shellfish Poisoning by Liquid Chromatography-Tandem Mass Spectrometry)

  • 이가정;스즈키 도시유키;김풍호;오은경;송기철;김지회
    • 한국식품과학회지
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    • 제41권4호
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    • pp.458-463
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    • 2009
  • 설사성패류독의 신속정밀 분석조건 확립을 위하여 LC-MS/MS를 사용하여 이동상, 분석용 column 및 collision energy 등을 변화시키면서 시험하였다. 50 mM formic acid와 2 mM ammonium formate가 함유된 acetonitrile 수용액을 이동상으로 사용하였을 때 OA와 DTX1이 검출되었다. Collision energy는 독소 성분에 따라 달리하는 것이 다성분 동시분석에 적합하였으며 OA와 DTX1 고유의 fragment ion들은 48 V 정도에서 최적의 intensity로 확인되었다. Column의 종류에 따라서는 $C_8$ column의 경우 OA, DTX1, DTX3, PTX2 및 YTX 모두 검출 가능하였으나 실제 검출 대상이 OA와 DTX1인 경우에는 일반적으로 사용되는 $C_{18}$ column도 적합한 것으로 확인되었다. 본 연구에서 확립한 LC-MS/MS 분석 조건의 검출한계는 OA와 DTX1 모두 1 ng/g, 정량한계는 각각 3 ng/g이었고, 표준독 성분을 첨가한 시료에서 process efficiency는 굴의 경우 91-118%, 진주담치에서는 96-117%이었고, matrix의 영향은 거의 없었다. 마우스 시험에서 양성을 나타낸 시료를 LCMS/MS법으로 분석한 결과, 일부 시료에서만 OA 및 DTX1이 검출되어 두 시험법의 독성은 일치하지 않았으며 LC-MS/MS법은 마우스 시험법보다 하루 이상 분석시간을 단축할 수 있었다.

PAHs 농도 분포에 따른 GC/MS와 HPLC의 분석특성에 관한 연구 (Analytical Characteristics of GC/MS and HPLC according to the Concentration Distribution of PAHs)

  • 홍좌령;최광민
    • 한국산업보건학회지
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    • 제25권3호
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    • pp.312-321
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    • 2015
  • Objectives: The purpose of this study was to determine the best method to analyze PAHs at extremely low concentrations. To this end, 16 PAHswere analyzed simultaneously by GC/MS, HPLC/FLD and HPLC/UVD, and the analytical characteristics of HPLC and GC/MS were compared. Methods: This study was conducted by GC/MS and HPLC/FLD/UVD, and evaluated linearity, precision and detection limit. Standard solutions were prepared for 21 samples in the range of $0.00001{\sim}1.0{\mu}g/mL$ and the samples were divided into four groups. All samples were made in three sets and analysis was replicated seven times. Results: Sixteen PAHs could be simultaneously separated by HPLC and GC/MS, and the adequate equipment was HPLC/FLD. The retention times by HPLC were shorter than GC/MS, and HPLC had better separation for most PAHs than GC/MS. The peaks of naphthalene and naphthalene-D8 partially overlapped for GC/MS. HPLC/FLD had a 20-2000 times lower limit of detection than GC/MS and UVD. However FLD was not adequate for analyzing acenaphthylene because it has too low a fluorescence quantum yield to be detected. The precision of HPLC/FLD/UVD and GC/MS showed less than 20% at $0.001{\mu}g/mL$ PAHs and when the concentration was higher, the coefficient of variation was decreased. HPLC/FLD was better for the overall detection of limits. Conclusions: The results indicate that the HPLC/FLD method has good linear range, precision and a detection of limits from $0.00001{\sim}0.0001{\mu}g/mL$ for all 16 PAHs. This study contributes to providing useful data for analysis technology and can be applied to occupational exposure measurement for PAHs in workplaces.

HPLC-MS/MS에 의한 사물탕의 지표성분 분석 (Analysis of Marker Substances in Samul-tang by HPLC-MS/MS)

  • 유영법;김미정;황대선;하혜경;마진열;신현규
    • 대한본초학회지
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    • 제22권2호
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    • pp.97-102
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    • 2007
  • Objectives : This study presents a high performance liquid chromatography - electrospray ionization-mass spectrometer (HPLC-MS/MS) methods for the quantitative and qualitative analysis of various active components in Samul-tang, which is composed of four crude herbs. Methods : HPLC-ESI-MS/MS for the determinations of paeoniflorin and 5-HMF (5-hydroxymethyl 2-furaldehyde) in the Samul-tang, the separation method was performed on an COSMOS1L 5C18-AR-Il (2.0 X 150 mm I.D.) column by gradient elution with 0.1% acetic acid and 5% CH3CN in water (A)-0.1% acetic acid and 5% H20 in CH3CN (B) as the mobile phase at a flow-rate of 300 ${\mu}L/min$ with detection at quadrupole mass spectrometer. The all marker substances were always detected as the base peaks in the positive ion mode. Results : The paeoniflorin of Paeoniae Radix in Samul-tang showed a strong base peak [M+H2O]+ in the positive detection mode to give the following as; paeoniflorin (498.109 [M+H2O]+, 479.8 [M]+, 301 [M-glucose]+, 179.3 [glucose]+). Based on the HPLC retnetion time and MS of standard compounds confirmed the identity of active compounds in Rehmanniae Radix Preparata as follows; 5-HMF (127.0[M+H]+, 109.3 [M-OH]+) in the positive ion mode. Conclusion : According to the above results, HPLC-ESI-MS method permits assignment of tentative structures such as paeoniflorin and 5-HMF in the Samul-tang.

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LC-MS/MS를 이용한 패류 및 피낭류 중 마비성 패류독소 분석법의 유효성 검증 (Validation of LC-MS/MS Method for Analysis of Paralytic Shellfish Toxins in Shellfish and Tunicates)

  • 조성래;김동욱;유헌재;조성해;류아라;이가정;목종수
    • 한국수산과학회지
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    • 제53권2호
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    • pp.174-180
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    • 2020
  • The mouse bioassay has been used widely for the monitoring of paralytic shellfish toxins (PSTs) in many countries. However, this method shows low sensitivity and high limit of detection (LOD), as well as it cannot confirm toxic profiles. Recently, LC-MS/MS method was studied for the quantitative of PSTs, however, the method has any problems with unstable retention times by ionization suppression caused by high salt concentration in shellfish extracts. To establish an alternative method for PSTs analysis, we tried to original LC-MS/MS methods adding desalting operation using amorphous graphitized polymer carbon solid-phase extraction cartridges. The method validation was conducted to determine linearity, limit of detection, limit of quantification (LOQ), accuracy, and precision in quantifying PSTs. The correlation coefficients for all tested PSTs maintained over 0.999. The LODs and LOQs for all PSTs were about 0.19-1.05 ㎍/kg and 0.58-3.18 ㎍/kg, respectively. The accuracies for PSTs were 95.4-107.7% for saxitoxin group, 97.1-100.9% for gonyautoxin group, 99.0-100.8% for N-sulfocarbamoyl toxin group, and 96.8-104.6% for decarbamoyl toxin group. These results indicate that the modified LC-MS/MS method was appropriate for analyzing the PSTs in shellfish and tunicates.

열분해/GC/MS와 IR을 이용한 사찰 벽화 시편 교착제 분석 (Analysis of Binding Media Used in Mural Painting of Temple Wall by Pyrolysis/GC/MS and IR)

  • 박종서;이정원
    • 보존과학회지
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    • 제33권5호
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    • pp.345-354
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    • 2017
  • 전남 진도군 소재 사찰의 보수 공사 중 벽화가 발견되어 제작기법 파악을 위해 교착제로 사용된 물질을 확인하고자 하였다. 이에 해당 벽화 시편에 대해 열분해/GC/MS와 IR 분석을 실시하였으며, 열분해/GC/MS분석은 직접 열분해와 온라인 메틸화법을 도입하였다. IR 분석에서 아교, 옻, 황칠 등 전통 교착제와 초산아크릴계 수지의 스펙트럼을 벽화시편과 비교했을 때 유사하지 않았으며, 건성유인 아마인유와 비교했을 때도 유사도가 낮았다. 벽화시편의 열분해/GC/MS 분석 결과를 옻, 황칠, 아교, 초산아크릴수지와 비교했을 때 이들 물질이 아닌 것으로 나타났다. 한편, 벽화시편에서 팔미트산, 옥타데칸산, nonanedioic acid, 옥타데센산 등 건성유에 특징적인 물질이 검출되었고, 경화 건성유와 유사한 열분해/GC/MS 크로마토그램이 관찰되었다. 따라서, 벽화는 건성유를 교착제로 사용하여 제작된 것으로 판단되었다.

Analysis of erectile dysfunction drugs and their analogues in counterfeit drugs and herbal medicines by LC-ESI-MS/MS

  • Lee, Ji Hyun;Jeong, Ji Hye;Park, Hyoung-Joon;Do, Jung Ah;Heo, Seok;Cho, Sooyeul;Yoon, Chang-Yong
    • 분석과학
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    • 제29권4호
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    • pp.155-161
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    • 2016
  • Distribution of various illegal or counterfeit drugs of seven approved erectile dysfunction drugs and their analogues has been increased, causing health problems such as cardiovascular disorder, tachycardia, headache, or vision disturbance. We used liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) to determine the erectile dysfunction drugs and their analogues in various counterfeit drugs. Eleven erectile dysfunction drugs and their analogues were detected, with sildenafil and its analogues being the most counterfeited compounds (73.8 %), followed by tadalafil and its analogues (25.4 %). The limits of detection (LOD) and the limits of quantitation (LOQ) of liquid-type and solid-type negative samples ranged from 0.1 to 3.3 ng/mL or ng/g and from 0.3 to 10.0 ng/mL or ng/g, respectively. The recoveries ranged from 84.3 to 112.3 % and 83.2 to 110.2 %, respectively. The contents of sildenafil and tadalafil in the various counterfeit drugs ranged from 21.0 to 947.5 mg/g and from 0.2 to 170.2 mg/g, respectively.

Characterization of the N-glycosylation of Recombinant IL-4 and IL-13 Proteins Using LC-MS/MS Analysis and the I-GPA Platform

  • Lee, Ju Yeon;Choi, Jin-woong;Bae, Sanghyeon;Hwang, Heeyoun;Yoo, Jong Shin;Lee, Joo Eon;Kim, Eunji;Jeon, Young Ho;Kim, Jin Young
    • Mass Spectrometry Letters
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    • 제12권3호
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    • pp.66-75
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    • 2021
  • Interleukin-4 (IL-4) and IL-13 are cytokines secreted by immune cells. Cytokines induce the proliferation of macrophages or promote the differentiation of secretory cells. The initiation and progression of allergic inflammatory diseases, such as asthma, are dependent on cytokines acting through related receptor complexes. IL-4 and IL-13 are N-glycoproteins. Glycan structures in glycoproteins play important roles in protein folding, protein stability, enzymatic function, inflammation, and cancer development. Therefore, the glycan structure of IL-4 and IL-13 needs to be elucidated in detail for the development of effective therapies. We report the first attempt to characterize the site-specific N-glycosylation of recombinant IL-4 and IL-13 via liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. The tandem mass spectra of intact N-glycopeptides were identified using the Integrated GlycoProteome Analyzer (I-GPA) platform, which can automatically and rapidly analyze multiple N-glycopeptides, including their glycan composition and amino acid sequences. The recombinant IL-4 and IL-13 were identified with amino acid sequence coverages of 84% and 96%, respectively. For IL-4, 52 glycoforms on one N-glycosylation site were identified and quantified. In IL-13, 232 N-glycopeptides from three N-glycosylation sites were characterized, with the site Asn52 being the most extensively glycosylated (~80%). The complex glycans were the most abundant glycan on IL-4 and IL-13 (~96% and 91%, respectively), and the biantennary glycans were the most abundant in both recombinant IL-4 and IL-13 proteins.