• 제목/요약/키워드: limit of quantification

검색결과 464건 처리시간 0.03초

Quantification of Fargesin in Mouse Plasma Using Liquid Chromatography-High Resolution Mass Spectrometry: Application to Pharmacokinetics of Fargesin in Mice

  • Lee, Min Seo;Lim, Chang Ho;Bang, Young Yoon;Lee, Hye Suk
    • Mass Spectrometry Letters
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    • 제13권1호
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    • pp.20-25
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    • 2022
  • Fargesin, a tetrahydrofurofuranoid lignan isolated from Flos Magnoliae, shows anti-inflammatory, anti-oxidative, anti-allergic, and anti-hypertensive activities. To evaluate the pharmacokinetics of fargesin in mice, a sensitive, simple, and selective liquid chromatography-high resolution mass spectrometric method using electrospray ionization and parallel reaction monitoring mode was developed and validated for the quantification of fargesin in mouse plasma. Protein precipitation of 6 µL mouse plasma with methanol was used as sample clean-up procedure. The standard curve was linear over the range of 0.2-500 ng/mL in mouse plasma with the lower limit of quantification level at 0.2 ng/mL. The intra- and inter-day coefficient variations and accuracies for fargesin at four quality control concentrations including were 3.6-11.3% and 90.0-106.6%, respectively. Intravenously injected fargesin disappeared rapidly from the plasma with high clearance values (53.2-55.5 mL/min/kg) at 1, 2, and 4 mg/kg doses. Absolute bioavailability of fargesin was 4.1-9.6% after oral administration of fargesin at doses of 1, 2, and 4 mg/kg to mice.

아세틸아세톤 유도체화 시약과 HPLC를 이용한 미량 포름알데하이드 수질분석 (Determination of Trace Amounts of Formaldehyde in Water Using High Performance Liquid Chromatography and Acetylacetone as a Derivative Reagent)

  • 이기창;박재형;이원태
    • 대한환경공학회지
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    • 제37권2호
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    • pp.81-86
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    • 2015
  • 수중에 존재하는 포름알데하이드(formaldehyde)를 ${\mu}g/L$ 단위 농도까지 정량할 수 있는 간단한 분석법을 개발하였다. 시료 전처리시 유도체화 시약으로 아세틸아세톤(acetylacetone)을 사용하였고, 기존 분석방법과 달리 추출 및 농축과정을 거치지 않는 것이 장점이다. 시료에 유도체화 시약을 첨가하고 $80^{\circ}C$에서 30분 반응시킨 후 HPLC를 이용하여 포름알데하이드를 분석하였다. 본 방법에 대한 정도보증 결과, 방법검출한계 및 정량한계는 각각 1.6, $5.0{\mu}g/L$로 기존 분석법에 비하여 낮았다. 정밀도 및 정확도는 각각 0.6~3.0%, 91.6~106.3%로 우수하였다. 또한 다양한 환경시료에 대한 회수율 검증에서도 92.0~115.2%로 양호하게 나타났다.

Liquid Chromatography-tandem Mass Spectrometry for Quantification of Dioscin in Rat Plasma

  • Kong, Tae Yeon;Ji, Hye Young;Choi, Sang-Zin;Son, Miwon;Lee, Hye Suk
    • Mass Spectrometry Letters
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    • 제4권3호
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    • pp.55-58
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    • 2013
  • Dioscin is a biologically active steroidal saponin with anticancer and hepatoprotective effects. A rapid, selective, and sensitive liquid chromatographic method with electrospray ionization tandem mass spectrometry was developed for the quantification of dioscin in rat plasma. Dioscin was extracted from rat plasma using ethyl acetate at acidic pH. The analytes were separated on a Halo C18 column using gradient elution of acetonitrile and 0.1% formic acid and detected by tandem mass spectrometry in selected reaction monitoring mode. The standard curve was linear ($r^2$ = 0.998) over the concentration range of 1-100 ng/mL. The lower limit of quantification was 1.0 ng/mL using 50 ${\mu}L$ of plasma sample. The coefficient of variation and relative error for intra- and inter-assay at four QC levels were 1.3 to 8.0% and -5.4 to 10.0%, respectively. This method was applied successfully to the pharmacokinetic study of dioscin after oral administration of dioscin at a dose of 29.2 mg/kg in male Sprague-Dawley rats.

LC-MS/MS와 GC-MS를 이용한 세신 추출물 중 7종 성분의 함량분석 (Quantitative Analysis of the Seven Marker Components in Asarum sieboldii using the LC-MS/MS and GC-MS)

  • 서창섭;신현규
    • 생약학회지
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    • 제44권4호
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    • pp.350-361
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    • 2013
  • Asarum sieboldii has been used for treatment of fever, pain, common cold, and chronic sinusitis in Korea. In this study, we performed quantification analysis of seven major constituents including aristolochic acid I, aristolochic acid II, ${\alpha}$-asarone, ${\beta}$-asarone, elemicin, methyl eugenol, and safrole in the 70% ethanol extract of Asarum sieboldii and its solvent fractions, n-hexane, ethylacetate, n-butanol, and water ones using a ultra-performance liquid chromatography-electrospray ionization-mass spectrometer(UPLC-ESI-MS) and gas chromatography-mass spectrometer(GC-MS). Regression equations of seven components were acquired with $r^2$ values >0.99. The values of limit of detection(LOD) and quantification(LOQ) were 0.1-3.9 ng/mL and 0.3-11.7 mg/mL, respectively. The amount of the seven compounds in Asarum sieboldii were not detected -143.66 mg/g. The established LC-MS/MS and GC-MS methods will be helpful to improve quality control of Asarum sieboldii.

Isotope-Dilution Mass Spectrometry for Quantification of Urinary Active Androgens Separated by Gas Chromatography

  • Lee, Su-Hyeon;Choi, Man-Ho;Lee, Won-Yong;Chung, Bong-Chul
    • Mass Spectrometry Letters
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    • 제1권1호
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    • pp.29-32
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    • 2010
  • Cross reacting antibodies can cause an overestimation of the results of immunoassays. Therefore, alternative methods are needed for the accurate quantification of steroids. Gas chromatography combined with isotope-dilution mass spectrometry (GC-IDMS) is developed to quantify urinary active androgens, testosterone, epitestosterone and dihydrotestosterone, which are clinically relevant androgens to both hair-loss and prostate diseases. The method devised involves enzymatic hydrolysis with $\beta$-glucuronidase, solid-phase extraction, liquid-liquid extraction using methyl tert-butyl ether and subsequent conversion to pentafluorophenyldimethylsilyl-trimethylsilyl (flophemesyl-TMS) derivatives for sensitive and selective analysis in selected-ion monitoring mode. Flophemesyl-TMS derivatization not only eliminates matrix interference but also has a good peak resolution within a 6 min-run. A selective and sensitive GC technique with flophemesyl-TMS derivatives also allows accurate quantitative analysis of three active androgens when combined with IDMS. The limit of quantification of the three analytes was <50 pg/mL, and extraction recoveries ranged from 91.9 to 102.1%. The precision and accuracy were 1.2~6.5% and 89.0~106.7%, respectively. This GC-IDMS method can be useful for evaluating the drug efficacy and monitoring the biological processes responsible for male-pattern baldness and prostate diseases.

Uncertainty quantification based on similarity analysis of reactor physics benchmark experiments for SFR using TRU metallic fuel

  • YuGwon Jo;Jaewoon Yoo;Jong-Hyuk Won;Jae-Yong Lim
    • Nuclear Engineering and Technology
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    • 제56권9호
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    • pp.3626-3643
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    • 2024
  • One of the issues in the development of the sodium-cooled fast reactor (SFR) using transuranic (TRU) metallic fuel is the absence of criticality benchmark experiment that faithfully mocks up the nuclear characteristics of the target design for validation of the reactor core design code and its uncertainty quantification (UQ). This study aims to quantify the criticality uncertainty of a typical TRU burner with metallic fuel by using the standard upper safety limit (USL) estimation framework based on the similarity analysis of existing benchmark experiments but elaborated in two aspects:1) application of two-sided rather than one-sided tolerance interval and 2) inclusion of additional uncertainty to account for fission products and minor actinides not included in the benchmark experiments. To conduct the similarity analysis and evaluate the nuclear-data induced uncertainty, existing, well-verified computing codes were integrated, including the nuclear data sampling code SANDY, the nuclear data processing code NJOY, and the continuous-energy Monte Carlo code McCARD. Finally, using the SFR benchmark database comprising both publicly available and proprietary benchmark experiments, the criticality uncertainty of the TRU core model with metallic fuel was evaluated.

Bioavailability of chlorphenesin carbamate in human plasma using a simple HPLC.

  • Jeong, Ji-Hoon;Park, Joon-Hong;Choi, Tae-Sik;Lee, Dong-Kyu;Kang, Hee-Yun;Son, Byung-Hyuk;Sohn, Uy-Dong
    • 대한약학회:학술대회논문집
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    • 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.1
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    • pp.305.2-306
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    • 2003
  • We aimed at determining bioavailability of chlorphenesin carbamate, a muscle relaxant, and developing a simple analysis in human blood using HPLC. A rapid and sensitive HPLC method was developed and validated using reverse-phase C 18 column with retention time and limit of quantification of toferisone being 8.6 min and 0.5 ng/$m\ell$, respectively. Quantification was performed at 260 nm with tolferison as internal standard. (omitted)

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Bioavailability of tolperisone in human plasma using a simple HPLC.

  • Jeong, Ji-Hoon;Park, Joon-Hong;Choi, Tae-Sik;Lee, Dong-Kyu;Jung, Chan-Heon;Son, Byung-Hyuk;Sohn, Uy-Dong
    • 대한약학회:학술대회논문집
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    • 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.1
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    • pp.304.1-304.1
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    • 2003
  • We aimed at determining bioavailability of tolperisone, a muscle relaxant. and developing a simple analysis in human blood using HPLC. A rapid and snsitive HPLC method was developed and validated using reverse-phase C18 column with retention time and limit of quantification of toferisone being 7.3 min and 20 ng/$m\ell$, respectively. Quantification was performed at 260 nm with chlorphenesin as internal standard. (omitted)

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Bioavailability of Procainamide HCl in human plasma using a simple HPLC

  • Park, Joon-Hong;Jeong, Ji-Hoon;Choi, Tae-Sik;Lee, Dong-Kyu;Shim, Jae-Ho;Sohn, Uy-Dong
    • 대한약학회:학술대회논문집
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    • 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2-2
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    • pp.240.2-240.2
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    • 2003
  • We aimed at determining bioavailability of procainarnide HCl, an antiarrhythmic drug, and developing a simple analysis in human blood using HPLC. A rapid and sensitive HPLC method was developed and validated using reverse-phase C18 column with retension time and limit of quantification of procainamide HCl being 2.58 min and 50ng/ml, respectively. Quantification was performed at 275 nm with caffeine as internal standard. The method involved a simple extraction. In order to study blood level profile in time, eight volunteers were enrolled and orally took 250 mg procainamide HCl once. (omitted)

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Bioavailability of Clonazepam in human plasma using a simple HPLC

  • Lee, Dong-Kyu;Jeong, Ji-Hoon;Park, Joon-Hong;You, Dae-Sik;Sohn, Uy-Dong
    • 대한약학회:학술대회논문집
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    • 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2-2
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    • pp.244.1-244.1
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    • 2003
  • We aimed at determining bioavailability of clonazepam, an anxiolytic drug, and developing a simple analysis in human blood using HPLC. A rapid and sensitive HPLC method was developed and validated using reverse-phase C18 column with retension time and limit of quantification of clonazepam being 2.58 min and 5hg/ml, respectively. Quantification was performed at 235 nm with p-hydroxybenzoic acid ethyl ester as internal standard. The method involved a simple extraction. In order to study blood level profile in time, sight volunteers were enrolled and orally took 6 mg clonazepam once. (omitted)

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