• 제목/요약/키워드: ESI

검색결과 647건 처리시간 0.029초

Rapid Identification of Radical Scavenging Compounds in Blueberry Extract by HPLC Coupled to an On-line ABTS Based Assay and HPLC-ESI/MS

  • Kim, Chul-Young;Lee, Hee-Ju;Lee, Eun-Ha;Jung, Sang-Hoon;Lee, Dong-Un;Kang, Suk-Woo;Hong, Sae-Jin;Um, Byung-Hun
    • Food Science and Biotechnology
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    • 제17권4호
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    • pp.846-849
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    • 2008
  • This study employed high performance liquid chromatography (HPLC) coupled to an on-line $ABTS^+$ radical scavenging detection (RSD) system along with HPLC-electro spin impact/mass spectrometry (ESI/MS), to rapidly determine and identify antioxidant compounds occurring in blueberry extract. The extract was separated by HPLC, and then the radical scavenging activities of the separated compounds were evaluated by the on-line coupled $ABTS^+$-RSD system. The negative peaks of the $ABTS^+$-RSD system, which indicates the presence of antioxidant activity, were monitored by measuring the decrease in absorbance at 734 nm. The active components in the blueberry extract were identified by HPLC-ESI/MS using their MS spectra and retention times. According to the data acquired from the on-line HPLC-$ABTS^+$-based assay and HPLC-ESI/MS systems, the antioxidant compounds detected in the blueberry extract were identified as chlorogenic acid and 11 anthocyanins.

Identification of IY81149 and Its Metabolites in the Rat Plasma Using the On-Line HPLC/ESI Mass Spectrometry

  • Myung, Seung-Woon;Min, Hye-Ki;Jin, Chang-Bae;Kim, Myung-Soo;Lee, Seung-Mok;Chung, Gi-Ju;Park, Seong-Jun;Kim, Dong-Yeon;Cho, Hyun-Woo
    • Archives of Pharmacal Research
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    • 제22권2호
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    • pp.189-193
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    • 1999
  • Reversed-phase high-performance liquid chromatography/mass spectrometry (HPLC/MS) with an eletcrospray ionization (ESI) interface was applied to the identification of metabolites of IY81149 in the rat plasma. Fragments obtained using collision-induced dissociation (CID) in both positive and negative modes were utilized to elucidate the structure of metabolites. The eluent from the conventional HPLC column was split and directly introduced into an ESI-mass spectrometer for the identification of the structures. the CID technique allowed the sensitive identification of sulfonyl-IY81149 and hydroxy-IY81149 from the rat plasma.

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중증도 분류 간호사에 의한 응급환자 중증도 분류 신뢰도 측정 연구: Emergency Severity Index Version 4를 중심으로 (Reliability of the Emergency Severity Index Version 4 Performed by Trained Triage Nurse)

  • 최희강;최민진;김주원;이지연;신선화;이현정
    • 중환자간호학회지
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    • 제5권2호
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    • pp.61-71
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    • 2012
  • Purpose: The aim of this study was to measure the inter-rater reliability of Emergency severity index (ESI) version 4 among triage nurse. Methods: This study was carried out from August 11, 2010 to September 7, 2010 in a regional emergency department. Data collection was done by ten triage nurses who trained ESI v.4. Two research nurses and ten triage nurses scored the ESI version 4 to the patients as references, independently. We calculated the weighted kappa between the triage nurses and research nurses to evaluate the consistency of the ESI v.4. Results: A total of 233 patients were enrolled in this study. Classification of ESI level was as follows - level 1 (0.4%), level 2 (21.0%), level 3 (67.8%), level 4 (9.4%), and level 5 (1.3%). Inter-rater reliability by weighted kappa was 0.79 (95% Confidence Interval= 0.74-0.83) and agreement rate was 87.1%. Under-triage rate by triage nurse was 6.0% and over-triage rate was 6.9%. Conclusion: For this study, inter-rater reliability was measured good level between triage nurses and research nurses in Korean single ED.

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Unintentional lumbar facet joint injection guided by fluoroscopy during interlaminar epidural steroid injection: a retrospective analysis

  • Kim, Min Jae;Choi, Yun Suk;Suh, Hae Jin;Kim, You Jin;Noh, Byeong Jin
    • The Korean Journal of Pain
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    • 제31권2호
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    • pp.87-92
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    • 2018
  • Background: An epidural steroid injection (ESI) is a commonly administered procedure in pain clinics. An unintentional lumbar facet joint injection during interlaminar ESI was reported in a previous study, but there has not been much research on the characteristics of an unintentional lumbar facet joint injection. This study illustrated the imaging features of an unintentional lumbar facet joint injection during an interlaminar ESI and analyzed characteristics of patients who underwent this injection. Methods: From December 2015 to May 2017, we performed 662 lumbar ESIs and we identified 24 cases (21 patients) that underwent a lumbar facet joint injection. We gathered data contrast pattern, needle approach levels and directions, injected facet joint levels and directions, presence of lumbar spine disease as seen on magnetic resonance images (MRI), and histories of lumbar spine surgeries. Results: The contrast pattern in the facet joint has a sigmoid or ovoid contrast pattern confined to the vicinity of the facet joint. The incidence of unintentional lumbar facet joint injection was 3.6%. The mean age was 68.47 years. Among these 21 patients, 14 (66.7%) were injected in the facet joint ipsilaterally to the needle approach. Among the 20 patients who received MRI, all (100%) had central stenosis and 15 patients (75%) had severe stenosis. Conclusions: When the operator performs an interlaminar ESI on patients with central spinal stenosis, the contrast pattern on the fluoroscopy during interlaminar ESI should be carefully examined to distinguish between the epidural space and facet joint.

Quantitative Evaluation of Radix Astragali through the Simultaneous Determination of Bioactive Isoflavonoids and Saponins by HPLC/UV and LC-ESI-MS/MS

  • Kim, Jin-Hee;Park, So-Young;Lim, Hyun-Kyun;Park, Ah-Yeon;Kim, Ju-Sun;Kang, Sam-Sik;Youm, Jeong-Rok;Han, Sang-Beom
    • Bulletin of the Korean Chemical Society
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    • 제28권7호
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    • pp.1187-1194
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    • 2007
  • The three major active isoflavonoids (calycosin-7-O-β -glucoside, isomucronulatol 7-O-β-glucoside, formononetin) and two main saponins (astragaloside I, astragaloside IV) in an extract of Radix Astragali were determined using rapid, sensitive, reliable HPLC/UV and LC-ESI-MS/MS methods. The separation conditions employed for HPLC/UV were optimized using a phenyl-hexyl column (4.6 × 150 mm, 5 μm) with the gradient elution of acetonitrile and water as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 230 nm. The specificity of the peaks was determined using a triple quadrupole tandem mass spectrometer equipped with an electrospray ionization (ESI) source that was operated in multiple reaction monitoring (MRM) in the positive mode. These methods were fully validated with respect to the linearity, accuracy, precision, recovery and robustness. The HPLC/UV method was applied successfully to the quantification of three major isoflavonoids in the extract of Radix Astragali. The results indicate that the established HPLC/UV and LC-ESI-MS/MS methods are suitable for the quantitative analysis and quality control of multi-components in Radix Astragali.

HPLC/ESI-MS/MS에 의한 먹는물(정수) 중 의약물질의 분석 (The analysis of pharmaceuticals in drinking water by HPLC/ESI-MS/MS)

  • 박미선;김병주;명승운
    • 분석과학
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    • 제23권5호
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    • pp.457-464
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    • 2010
  • 먹는물(정수) 중에 잔류하는 버지니아마이신을 비롯한 macrolide 계열 의약물질 3종과 시메티딘을 동시에 정량 및 정성 분석하는 방법을 확립하였다. HLB 카트리지를 사용하여 분석물질을 추출/정제 및 농축한 후, HPLC/ESI-MS/MS를 이용하여 4종의 물질들을 효과적으로 분리하고 감도 좋게 검출할 수 있었다. 정량분석을 위해서 0.01~2.0 ng/mL 범위에서 $r^2$=0.995이상의 높은 직선성을 나타내는 검량선을 얻었으며, 시메티딘(37.7~48.1%)을 제외한 macrolide 계열 3종 의약물질은 64.7~118.1% 범위의 양호한 회수율을 나타내었다. 바탕 정수에 소량 첨가하여 얻은 분석방법의 검출한계와 정량한계는 각각 1.6~74.8 pg/mL 와 5.5~249.7 pg/mL 범위의 높은 감도를 나타내었다.

LC-ESI-MS/MS를 이용한 평위산 주요 성분의 함량 분석 (Quantitative Determination of the Marker Components in Pyungwi-San Using LC-ESI-MS/MS)

  • 서창섭;신현규
    • 생약학회지
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    • 제49권3호
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    • pp.270-277
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    • 2018
  • Pyungwi-san has been used to treat the digestive system diseases, physconia, nausea, anorexia, and dyspepsia in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was optimized for simultaneous determination of the 14 marker components, spinosin, liquiritirn apioside, liquiritin, narirutin, 6'''-feruloylspinosin, hesperidin, liquiritigenin, glycyrrhizin, 6-gingerol, atractylenolide III, honokiol, atractylenolide II, magnolol, and atractylenolide I in Pyungwi-san extract. All analytes were separated on a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) with maintained at $45^{\circ}C$. The mobile phase consisted of 0.1% (v/v) aqueous formic acid and acetonitrile. The MS conditions were as follows: capillary voltage 3.3 kV, extractor voltage 3.0 V, RF lens voltage 0.3 V, source temperature $120^{\circ}C$, desolvation temperature $300^{\circ}C$, desolvation gas 600 L/h, cone gas 50 L/h and collision gas 0.14 mL/min. The coefficient of determination of 14 analytes was 0.9989-1.0000. The limits of detection and quantification values of the all analytes were 0.04-2.56 and 0.13-7.69 ng/mL, respectively. As a result of the analysis using the established LC-ESI-MS/MS method, the 5 components, spinosin, 6'''-feruloylspinosin, atractylenolide III, II, and I derived from Zizyphi Fructus and Atractylodis Rhizoma, were not detected in this extract. On the other hand, the 9 components except for the 5 components were 4.15-498.87 mg/kg in lyophilized Pyungwi-san extract. Among these components, glycyrrhizin, marker compound of Glycyrrhizae Radix et Rhizoma, was detected the most amount as a 498.87 mg/kg.

LC/ESI-MS/MS를 이용한 하천수 중 잔류 6종 의약물질의 동시분석 및 모니터링 (Simultaneous analysis and occurrences of six pharmaceuticals in surface water by LC/ESI-MS/MS)

  • 김병주;명승운
    • 분석과학
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    • 제23권6호
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    • pp.572-578
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    • 2010
  • 본 연구에서는 하천수 중 6종의 의약물질(cephradine, cefadroxil, penicillin G, vancomycin, iopromide, and fenbendazole)에 대한 전처리법과 분석 방법을 확립하였다. 하천수 중의 분석물질을 HLB(Hydrophilic-Lipophilic Balanced) 카트리지를 사용하여 추출/정제 및 농축하였다. HPLC/ESI-MS/MS를 이용하여 6종의 물질들을 동시에 분석하였다. Fenbendazole을 제외한 의약물질은 71.1~92.6% 범위의 양호한 회수율을 나타내었고, 상대표준편차는 11.2% 이하로 나타났다. 정량분석을 위해서 0.007~1.2 ng/mL 범위에서 $r^2$=0.99 이상의 높은 직선성을 나타내는 검량선을 얻었다. 검출한계(LOD)와 정량한계(LOQ)는 각각 7.2~128.7 pg/mL, 23.8~429.1 pg/mL로 나타났다. 이 분석 방법은 하천수 중 의약품에 대한 모니터링에 유용하며, 하천수 중 iopromide과 fenbendazole은 높은 농도로 검출되었다.

HPLC-ESI/MS/MS를 이용한 생양파와 흑양파의 퀘세틴 배당체 분석 (Quercetin Glucoside Profiling of Fresh Onion (Allium cepa) and Aged Black Onion Using HPLC-ESI/MS/MS)

  • 정동민;권선화;정영철;전효곤
    • 생명과학회지
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    • 제21권3호
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    • pp.464-467
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    • 2011
  • 퀘세틴은 양파에 있는 주요한 플라보노이드이고, 항산화제 역할을 한다. 양파에 있는 퀘세틴은 주로 배당체 형태로 존재한다. 흑양파는 습도 90%와 온도 $60^{\circ}C$ 조건 하에서 30일 동안의 숙성처리과정으로 만들어진다. 흑양파 제조과정 전후의 양파 속에 있는 퀘세틴과 퀘세틴 배당체들은 HPLC-ESI/MS/MS를 이용하여 분석되었다. 생양파 속에는 퀘세틴 단당체와 퀘세틴 이당체가 동정되었고, 반면에 흑양파 속에는 퀘세틴만이 존재하였다. 그러한 결과들은 생양파에 있는 퀘세틴 배당체(단당체와 이당체)들은 숙성과정 동안 해당과정이 일어난다는 것을 의미한다. 이러한 분석프로파일은 숙성과정 동안 발생되는 양파의 주요한 두 개의 퀘세틴 배당체들의 변화를 추정하는데 용이한 방법을 제공할 것이다.

LC/ESI-MS/MS를 이용한 식육(소, 돼지)중 잔류 phoxim 분석 (Analysis of Phoxim Residue in Animal Food Production (Cattle and Pig) by LC/ESI-MS/MS)

  • 박미선;이진주;명승운
    • 대한화학회지
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    • 제55권4호
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    • pp.626-632
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    • 2011
  • 폭심(phoxim)은 널리 사용되고 있는 구충제인 동물용의약품이다. 본 논문에서는 소와 돼지 근육에 잔류하는 폭심을 분석하기 위해서, 실리카 고체상과 아세토니트릴을 사용하여 추출/정제하였다. 분석을 위해서 LC/ESI-MS/MS 방법이 사용되었다. HPLC에서 $C_{18}$ 컬럼($2.1{\times}100\;mm$, $3.5\;{\mu}m$)이 사용되었으며, 이동상으로는 0.1% formic acid와 물이 사용되었다. 소(0.0048~2.0 mg/kg)와 돼지(0.0055~2.0 mg/kg)에 소량첨가하여 얻은 검정곡선은 좋은 직선성($r^2$=0.995)을 나타내었다. 소와 돼지의 매트릭스에 대해서 0.0048~0.2 mg/kg범위에서 68.2~106.9%의 정확도를 나타내었으며, LOD는 0.0014~0.0017 mg/kg, LOQ는 0.0048~0.0055 mg/kg범위에 있었으며, 11.2%의 상대표준편차를 나타내었다.