• Title/Summary/Keyword: Reaction monitoring

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Monitoring of Free Sugar and Amino Acid of Red Bean Paste by Corn Syrup Concentration and Heating Treatment Conditions (물엿농도와 열처리 조건에 따른 팥앙금 호화액의 당 및 아미노산의 변화 모니터링)

  • Rho, Min-Whan;Lee, Tae-Kyoo
    • Food Science and Preservation
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    • v.13 no.5
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    • pp.581-588
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    • 2006
  • Dynamic changes of free sugar and amino acid in the mixture of red bean paste sediment by corn syrup concentration and heating conditions were monitored. Glucose and fructose contents of red bean paste increased with an increasing blown color intensity. Amino acid content was affected by the heating temperature, increased with an increase in browning color intensify. Browning color intensity of each samples increased up to $95^{\circ}C$, but decreased above $95^{\circ}C$. This result was the same tend as changes of glucose and amino acid. The result of correlation coefficients among free sugar amino acid and browning color intensity show that increase in browning color intensity was not correlated directly with changes of free sugar and amino acid content. It seems that the contents of free sugar and amino acid resolved from saccharides and protein were much mote than contents nea for browning reaction.

Rapid Determination of Imatinib in Human Plasma by Liquid Chromatography-Tandem Mass Spectrometry: Application to a Pharmacokinetic Study

  • Yang, Jeong Soo;Cho, Eun Gi;Huh, Wooseong;Ko, Jae-Wook;Jung, Jin Ah;Lee, Soo-Youn
    • Bulletin of the Korean Chemical Society
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    • v.34 no.8
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    • pp.2425-2430
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    • 2013
  • A simple, fast and robust analytical method was developed to determine imatinib in human plasma using liquid chromatography-tandem mass spectrometry with electrospray ionization in the positive ion mode. Imatinib and labeled internal standard were extracted from plasma with a simple protein precipitation. The chromatographic separation was performed using an isocratic elution of mobile phase involving 5.0 mM ammonium formate in water-5.0 mM ammonium formate in methanol (30:70, v/v) over 3.0 min on reversed-stationary phase. The detection was performed using a triple-quadrupole tandem mass spectrometer in multiple-reaction monitoring mode. The developed method was validated with lower limit of quantification of 10 ng/mL. The calibration curve was linear over 10-2000 ng/mL ($R^2$ > 0.99). The method validation parameters met the acceptance criteria. The spiked samples and standard solutions were stable under conditions for storage and handling. The reliable method was successfully applied to real sample analyses and thus a pharmacokinetic study in 27 healthy Korean male volunteers.

Determination of Glimepiride in Human Plasma by Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry

  • Kim, Ho-Hyun;Chang, Kyu-Young;Lee, Hee-Joo;Han, Sang-Beom
    • Bulletin of the Korean Chemical Society
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    • v.25 no.1
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    • pp.109-114
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    • 2004
  • A sensitive method for quantitation of glimepiride in human plasma has been established using liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS). Glipizide was used as an internal standard. Glimepiride and internal standard in plasma sample was extracted using diethyl etherethyl acetate (1 : 1). A centrifuged upper layer was then evaporated and reconstituted with the mobile phase of acetonitrile-5 mM ammonium acetate (60:40, pH 3.0). The reconstituted samples were injected into a $C_{18}$ reversed-phase column. Using MS/MS in the multiple reaction monitoring (MRM) mode, glimepiride and glipizide were detected without severe interference from human plasma matrix. Glimepiride produced a protonated precursor ion ([M+H]$^+$) at m/z 491 and a corresponding product ion at m/z 352. And the internal standard produced a protonated precursor ion ([M+H]]$^+$) at m/z 446 and a corresponding product ion at m/z 321. Detection of glimepiride in human plasma by the LC-ESI/MS/MS method was accurate and precise with a quantitation limit of 0.1 ng/mL. The validation, reproducibility, stability, and recovery of the method were evaluated. The method has been successfully applied to pharmacokinetic studies of glimepiride in human plasma.

Review of Recent Smog Chamber Studies for Secondary Organic Aerosol (스모그 챔버를 이용한 이차 초미세유기먼지의 최근 연구 동향)

  • Lim, Yong Bin;Lee, Seung-Bok;Kim, Hwajin;Kim, Jin Young;Bae, Gwi-Nam
    • Journal of Korean Society for Atmospheric Environment
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    • v.32 no.2
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    • pp.131-157
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    • 2016
  • A smog chamber has been an effective tool to study air quality, particularly secondary organic aerosol (SOA), which is typically formed by atmospheric oxidation of volatile organic compounds (VOCs). In controlled environments, smog chamber studies have validated atmospheric oxidation by identifying, quantifying and monitoring products with state-of-art instruments (e.g., aerosol mass spectrometer, scanning mobility particle sizer) and provided chemical insights of SOA formation by elucidating reaction mechanisms. This paper reviews types of smog chambers and the current state of smog chamber studies that have accomplished to find pathways of SOA formation, focusing on gas-particle partitioning of semivolatile products of VOC oxidation, heterogeneous reactions on aerosol surface, and aqueous chemistry in aerosol waters (e.g., cloud/fog droplets and wet aerosols). For future chamber studies, then, this paper discusses potential formation pathways of fine particles that East Asia countries (e.g., Korea and China) currently suffer from due to massive formation that gives rise to fatal health problems.

Sensitive Determination of Pinaverium Bromide in Human Plasma by LC-ESI-MS/MS : Applicability to Oral Bioavailability Determination (LC-ESI-MS/MS를 이용한 생체시료 중 브롬화피나베리움의 고감도 분석 및 이를 이용한 생체이용률 평가)

  • Park, Seok;Lee, Ye-Rie;Kim, Ho-Hyun;Lee, Hee-Joo;Kim, Yoon-Gyoon;Youm, Jeong-Rok;Han, Sang-Beom
    • Journal of Pharmaceutical Investigation
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    • v.34 no.6
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    • pp.513-519
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    • 2004
  • A sensitive method for quantification of pinaverium bromide in human plasma was established using liquid chromatography-electrospray ionization tandem mass spectrometry(LC-ESI-MS/MS). Glimepiride was used as internal standard. Pinaverium bromide and internal standard in plasma sample were extracted using tert-butylmethylether(TBME). A centrifuged upper layer was then evaporated and reconstituted with mobile phase of acetonitrile-5 mM ammonium formate (80/20, pH 3.0). The reconstituted samples were injected into a $C_{18}$ reversed-phase column. Using MS/MS with multiple reaction monitoring (MRM) mode, pinaverium and glimepirde were detected without severe interference from human plasma matrix. Pinaverium produced a protonated precursor ion $([M+H]^+)$ at m/z 510.3 and a corresponding product ion at m/z 228.9. Internal standard produced a protonated precursor ion $([M+H]^+)$ at m/z 491.5 and a corresponding product ion at m/z 352.0. Detection of pinaverium bromide in human plasma was accurate and precise, with limit of quantitation at 0.5 ng/ml. The method has been successfully applied to bioavailability study of pinaverium bromide tablet in Korean healthy male volunteers. Pharmacokinetic parameters such as $AUC_t,\;C_{max},\;T_{max},\;K_{el}\;and\;t_{1/2}$ were calculated.

Identification of Pitfalls Related to the Analysis of Liquid Chromatography-Tandem Mass Spectrometry and Liquid Chromatography-Time of Flight Mass Spectrometry (액체크로마토그래프-질량분석기를 이용한 정성 및 정량 오류의 확인)

  • Kwon, Jin-Wook;Cho, Yoon-Jae;Rhee, Gyu-Seek
    • Korean Journal of Environmental Agriculture
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    • v.34 no.3
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    • pp.230-237
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    • 2015
  • BACKGROUND: To identify the sources of inaccuracy in LC/MS/MS methods used in the routine quantitation of small molecules are described and discussed. METHODS AND RESULTS: Various UPLC coupled to triple quadrupole mass spectrometer and time of flight (TOF) were used to identify the potential sources of inaccuracy and inducing the pitfalls of qualification and quntitation during the veterinary drug residue analysis. Some of stable isotope labelled veterinary drugs, which were used as internal standards, presented "cross-talk", regardless of manufactures of mass spectrometer and types of spectrometer. Group of sulfonamides also presented inaccuracy qualification and quantitation due to the multi-residue analytical method with the same fragment ions at the close retention times. CONCLUSION: The phenomena of "cross-talk" occurring between subsequently monitored transition from stable isotope labelled and isotope non-labelled authentic chemical were identified. To prevent errors and achieve more accurate data during the analysis of small molecules by LC/MS/MS SRM method, Followings should be taken care of and kept checking; purity and concentration of stable isotope as an internal standard, prevention of carry-over during the separation in column, minimizing the ion suppression by matrix effect, identification of retention time, precursor ion and product ion, and full knowledge of data processing including smoothing and peak integration.

A Study on Safety, Performance and Clinical effectiveness Test Guideline of Versatile Ophthalmic Laser System (다목적 안과용 레이저 시스템 안전성 성능평가 및 임상적 유효성평가 가이드라인 수립을 위한 연구)

  • Kim, You Rim;Yu, Woo Jin;Park, Ho Joon;Jang, Won Seuk
    • Journal of Biomedical Engineering Research
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    • v.40 no.6
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    • pp.250-259
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    • 2019
  • Ophthalmic Laser System is widely used in Selective Laser Trabeculoplasty of Open Angle Glaucoma and Ocular Hypertension. Versatile ophthalmic laser system is a medical device with technology that checks the condition of the treatment area by irradiating a continuous laser pulse on the treatment area, and monitoring the microbubble reaction caused by the temperature increase of the melanosome through the ultrasonic signal and the optical signal sensor. It performs selective laser treatment without damaging the photoreceptor by controlling the wavelength of the laser when microbubbles are detected. This study aims to suggest a guideline for evaluating safety, performance and clinical effectiveness of Versatile Ophthalmic Laser System in accordance with the growing technology. International Standards, Regulations, and Clinical Trial Protocols were investigated and analyzed for this study. As a result of this study, the safety, performance and clinical effectiveness test guideline for Versatile Ophthalmic Laser System were proposed. This guideline will ensure the safety and efficacy of Medical device, and furthermore it is expected to be able to promote the development of technology development by supporting a clinical trial plan.

Determination of Enantiopurity of Chiral Epoxides by Vibrational Circular Dichroism Spectroscopy (진동 원편광 이색성 분광기를 사용한 키랄 에폭사이드의 광학순도 분석)

  • Lee, Joo-Hyun;Lee, Choong-Young;Kim, Geon-Joong
    • Applied Chemistry for Engineering
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    • v.23 no.6
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    • pp.577-582
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    • 2012
  • In this work, vibrational circular dichroism (VCD) technique was applied for the determination of %EE of chiral compounds. It may provide an easy way to determine the %EE with a proper accuracy within 2% error ranges as well as the absolute configuration of enantiomers. We demonstrated herein a flow cell VCD (FT-VCD) technique for time-dependent %EE measurements. The simultaneous monitoring of the mole fraction and %EE for two chiral species (epichlorohydrin and glycidol mixture) in the mixture was shown to be successful without any further separation steps. Thus, we demonstrate that FT-VCD is an appropriate analytical tool to monitor the kinetics of reactions involving chiral molecules. FT-VCD also provides a convenient nondestructive approach for the time dependent determination of the optical purity of individual components in a reaction mixture containing chiral molecules.

Ultra-fast Generic LC-MS/MS Method for High-Throughput Quantification in Drug Discovery

  • Kim, So-Hee;Yoo, Hye Hyun;Cha, Eun-Ju;Jeong, Eun Sook;Kim, Ho Jun;Kim, Dong Hyun;Lee, Jaeick
    • Mass Spectrometry Letters
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    • v.4 no.3
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    • pp.47-50
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    • 2013
  • An ultra-fast generic LC-MS/MS method was developed for high-throughput quantification of discovery pharmacokinetic (PK) samples and its reliability was verified. The method involves a simple protein precipitation for sample preparation and the analysis by ultra-fast generic LC-MS/MS with the ballistic gradient program and selected reaction monitoring (SRM) mode. Approximately 290 new chemical entities (NCEs) (over 10,000 samples) from 5 therapeutic programs were analyzed. The calibration curves showed good linearity in the concentration range of 1, 2 or 5 to 2000 ng/mL. No significant ion suppression was observed in the elution region of all the NCEs. When approximately 300 plasma samples were continuously analyzed, the peak area of internal standard was constant and reproducible. In the repeated analysis of samples, the plasma concentrations and the area under the curve (AUC) were consistent with the results from the first analysis. These results showed that the present ultra-fast generic LC-MS/MS method is reliable in terms of selectivity, sensitivity, and reproducibility and could be useful for high-throughput quantification and other bioanalysis in drug discovery.

Simple and Rapid Liquid Chromatography-Tandem Mass Spectrometry Analysis of Arctigenin and its Application to a Pharmacokinetic Study

  • Thapa, Subindra Kazi;Weon, Kwon-Yeon;Jeong, Seok Won;Kim, Tae Hwan;Upadhyay, Mahesh;Han, Yo-Han;Jin, Jong-Sik;Hong, Seung-Heon;Youn, Yu Seok;Shin, Beom Soo;Shin, Soyoung
    • Mass Spectrometry Letters
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    • v.8 no.2
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    • pp.23-28
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    • 2017
  • Arctigenin is the main active ingredient of Fructus Arctii, which has been reported with a variety of therapeutic activities including anti-cancer, anti-inflammation, anti-virus, and anti-obesity effects. In this study, a simple and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the determination of arctigenin in rat plasma. The assay utilized a simple protein precipitation with methanol and the mobile phase consisted of 100% methanol and water containing 0.1% formic acid (65:35 v/v). Arctigenin and the internal standard (psoralen) were monitored using a positive electrospray turbo ionspray mode with multiple reaction monitoring transitions of m/z $373.2{\rightarrow}136.9$ and m/z $187.2{\rightarrow}130.9$, respectively, and total chromatographic run time was within 5 min. The lower limit of quantification (LLOQ) of arctigenin was 5 ng/mL in the rat plasma. The intra- and inter-day accuracy of arctigenin at LLOQ and matrix-matched quality control samples ranged 97.4 - 104.8% and 97.2 - 102.0%, respectively. The intra-day precision was within 4.80% and the inter-day precision was within 5.92%. Application of the present method was demonstrated through a pharmacokinetic study after intravenous and oral administration of arctigenin in male Sprague Dawley rats.