• Title/Summary/Keyword: Quantification Analysis

Search Result 1,448, Processing Time 0.032 seconds

Analysis of Benzene in Beverages by Headspace-GC/MS (Headspace-GC/MS를 이용한 음료 중 벤젠 분석)

  • Kim, Eun-Ju;Park, Sang-Aeh;Choi, Dong-Mi
    • Journal of Food Hygiene and Safety
    • /
    • v.22 no.4
    • /
    • pp.243-247
    • /
    • 2007
  • A selective analytical method of headspace-GC/MS has been applied to determine levels of benzene in beverages. Food samples were 85 including 2 fruit juices, 6 fruit beverages, 11 carbonated beverages, 55 mixed beverages, and 4 beverage concentrations, and 7 extracted beverages. For phase equilibration of headspace, sample was stirred at $40^{\circ}C$ for 30 min. The oven temperature was $60^{\circ}C$ and elevated to $180^{\circ}C$ at $15^{\circ}C/min$. The internal standard was benzene-d6. The identification was done by the selected target ions such as m/z 51, 77, and 78 and the confirmation was done by the response ratio of m/z 77 to m/z 78 between sample and standard. The overall recoveries were ranged from 91% to 101% and the limit of quantification was $1{\mu}g/kg$. The average level of benzene were $5{\mu}g/kg$ for fruit beverages, $2{\mu}g/kg$ for carbonated beverages, $7{\mu}g/kg$ for mixed beverages and $7{\mu}g/kg$ for extracted beverages.

Development and Validation of an HPLC Method for the Pharmacokinetic Study of Fexofenadine in Human (테르페나딘 체내동태 연구를 위한 혈청 중 펙소페나딘의 HPLC 정량법 개발 및 검증)

  • Cho, Hye-Young;Kang, Hyun-Ah;Kim, Yoon-Gyoon;Choi, Hoo-Kyun;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
    • /
    • v.35 no.6
    • /
    • pp.437-443
    • /
    • 2005
  • A rapid, selective and sensitive reversed-phase HPLC method for the determination of a major metabolite of terfenadine, fexofenadine, in human serum was developed, validated, and applied to the pharmacokinetic study of terfenadine. Fexofenadine and internal standard, haloperidol were extracted from human serum by liquid-liquid extraction with acetonitrile and analyzed on a $Symmetry^{TM}$ C8 column with the mobile phase of 1% triethylamine phosphate (pH 3.7)-acetonitrile (67:33, v/v, adjusted to pH 5.6 with triethylamine). Detection wavelength of 230 nm for excitation, 280 nm for emission and flow rate of 1.0 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^{3}$ factorial design using a fixed fexofenadine concentration (50 ng/mL) with respect to its peak area and retention time. In addition, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 10-500 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of serum was 10 ng/mL, which was sensitive enough for the pharmacokinetic studies of terfenadine. The overall accuracy of the quality control samples ranged from 95.70 to 114.58% for fexofenadine with overall precision (% C.V.) being 3.53-14.39%. The relative mean recovery of fexofenadine for human serum was 90.17%. Stability studies (freeze-thaw, short-term, extracted serum sample and stock solution) showed that fexofenadine was stable during storage, or during the assay procedure in human serum. However, the storage at $-70^{\circ}C$ for 4 weeks showed that fexofenadine was not stable. The peak area and retention time of fexofenadine were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of fexofenadine in human serum samples for the pharmacokinetic studies of orally administered Tafedine tablet (60 mg as terfenadine) at three different laboratories, demonstrating the suitability of the method.

Development and Validation of an HPLC Method for the Pharmacokinetic Study of Etodolac in Human (에토돌락 체내동태 연구를 위한 혈청 중 에토돌락의 HPLC 정량법 개발 및 검증)

  • Cho, Hea-Young;Kang, Hyun-Ah;Moon, Jai-Dong;Choi, Hoo-Kyun;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
    • /
    • v.35 no.4
    • /
    • pp.265-271
    • /
    • 2005
  • A rapid, selective and sensitive reversed-phase HPLC method for the determination of etodolac in human serum was developed, validated, and applied to the pharmacokinetic study of etodolac. Etodolac and internal standard, ibuprofen were extracted from human serum by liquid-liquid extraction with hexane/isopropanol (95:5, v/v) and analyzed on a Luna C18(2) column with the mobile phase of 1% aqueous acetic acid-acetonitrile (4:6, v/v). Detection wavelength of 227 nm and flow rate of 1.0 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^3$ factorial design using a fixed etodolac concentration $(1\;{\mu}g/mL)$ with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of $0.05-40\;{\mu}g/mL$ with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of serum was 0.05 ${\mu}g/mL$, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the quality control samples ranged from 92.00 to 110.00% for etodolac with overall precision (% C.V.) being 1.08-10.11%. The percent recovery for human serum was in the range of 76.73-115.30%. Stability studies showed that etodolac was stable during storage, or during the assay procedure in human serum. The peak area and retention time of etodolac were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of etodolac in human serum samples for the pharmacokinetic studies of orally administered Lodin XL tablet (400 mg as etodolac) at three different laboratories, demonstrating the suitability of the method.

ACAT (Acyl-CoA:cholesterol Acyltransferase) Inhibitory Effect and Quantification of Pyranocurmarin in Different Parts of Angelica gigas Nakai (참당귀(Angelica gigas)에서 분리한 pyranocurmarin 성분의 ACAT 저해활성 및 참당귀 부위별 pyranocurmarin 성분의 함량 분석)

  • Kim, Geum-Soog;Park, Chun-Geun;Jeong, Tae-Sook;Cha, Seon-Woo;Baek, Nam-In;Song, Kyung-Sik
    • Journal of Applied Biological Chemistry
    • /
    • v.52 no.4
    • /
    • pp.187-194
    • /
    • 2009
  • Two pyranocoumarin constituents have been isolated from Angelica gigas and were identified as decursinol angelate (1) and decursin (2) by means of NMR analysis, respectively. Human acyl-CoA:cholesterol acyltransferase (hACAT) inhibitory activity of decursinol angelate (1) and decursin (2) was evaluated. Decursin (2) showed significantly inhibitory activity against hACAT1 and hACAT2 with $IC_{50}$ value of 137 and $168\;{\mu}M$, respectively, whereas decursinol angelate (1) exhibited weak ACAT inhibitory activity. These results suggested that decusin from A. gigas might be effective for the prevention and the treatment of hypercholesterolemia or atherosclerosis by inhibitory effect on hACAT. The contents of decursinol angelate (1) and decursin (2) were analyzed in various parts of A. gigas including flower, seed, leaf and root using LC/MS/MS (ESI, positive ion mode, MRM mode). The content of decursinol angelate was increased in order of flower, seed, leaf, and root and decursin content was increased in order of flower, seed, leaf, and root. It was expected that unused parts including leaf and flower of A. gigas might be useful as new functional sources by their high contents of decursin and decursinol angelate.

Development and Validation of an HPLC Method for the Pharmacokinetic Study of Pentoxifylline in Human Serum (체내동태 연구를 위한 혈청 중 펜톡시필린의 HPLC 정량법 개발 및 검증)

  • Cho, Hea-Young;Kang, Hyun-Ah;Yoo, Hee-Doo;Lee, Hwa-Jeong;Moon, Jai-Dong;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
    • /
    • v.36 no.2
    • /
    • pp.89-95
    • /
    • 2006
  • A selective and sensitive reversed-phase HPLC method for the determination of pentoxifylline in human serum was developed, validated, and applied to the pharmacokinetic study of pentoxifylline. Pentoxifylline and internal standard, chloramphenicol, were extracted from the serum by liquid-liquid extraction with dichloromethane and analyzed on a Luna CI8(2) column with the mobile phase of acetonitrile-0.034 M phosphoric acid (25:75, v/v, adjusted to pH 4.0 with 10 M NaOH). Detection wavelength of 273 nm and flow rate of 0.8 mL/min were used. This method showed linear response over the concentration range of 10-500 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of the serum was 10 ng/mL, which was sensitive enough for pharmacokinetic studies of pentoxifylline. The overall accuracy of the quality control samples ranged from 89.3 to 92.7% for pentoxifylline with overall precision (% C.V.) being 4.1-9.2%. The relative mean recovery of pentoxifylline for human serum was 105.8%. Stability (stock solution, short and long-term) studies showed that pentoxifylline was not stable during storage. But three freeze-thaw cycles and extracted serum samples were stable. This method showed good ruggedness (within 15% C.V.) and was successfully applied for the analysis of pentoxifylline in human serum samples for the pharmacokinetic studies of orally administered $Trental^{\circledR}$ tablet (400 mg pentoxifylline), demonstrating the suitability of the method.

NecroX-5 protects mitochondrial oxidative phosphorylation capacity and preserves PGC1α expression levels during hypoxia/reoxygenation injury

  • Vu, Thi Thu;Kim, Hyoung Kyu;Le, Thanh Long;Nyamaa, Bayalagmaa;Song, In-Sung;To, Thanh Thuy;Nguyen, Quang Huy;Marquez, Jubert;Kim, Soon Ha;Kim, Nari;Ko, Kyung Soo;Rhee, Byoung Doo;Han, Jin
    • The Korean Journal of Physiology and Pharmacology
    • /
    • v.20 no.2
    • /
    • pp.201-211
    • /
    • 2016
  • Although the antioxidant and cardioprotective effects of NecroX-5 on various in vitro and in vivo models have been demonstrated, the action of this compound on the mitochondrial oxidative phosphorylation system remains unclear. Here we verify the role of NecroX-5 in protecting mitochondrial oxidative phosphorylation capacity during hypoxia-reoxygenation (HR). Necrox-5 treatment ($10{\mu}M$) and non-treatment were employed on isolated rat hearts during hypoxia/reoxygenation treatment using an ex vivo Langendorff system. Proteomic analysis was performed using liquid chromatography-mass spectrometry (LC-MS) and non-labeling peptide count protein quantification. Real-time PCR, western blot, citrate synthases and mitochondrial complex activity assays were then performed to assess heart function. Treatment with NecroX-5 during hypoxia significantly preserved electron transport chain proteins involved in oxidative phosphorylation and metabolic functions. NecroX-5 also improved mitochondrial complex I, II, and V function. Additionally, markedly higher peroxisome proliferator-activated receptor-gamma coactivator-$1{\alpha}$ ($PGC1{\alpha}$) expression levels were observed in NecroX-5-treated rat hearts. These novel results provide convincing evidence for the role of NecroX-5 in protecting mitochondrial oxidative phosphorylation capacity and in preserving $PGC1{\alpha}$ during cardiac HR injuries.

Analysis and Quantification of Seawater Infiltration by Wave Action in Coastal Zone (연안해역에서 파도에 의한 해수 침투이론의 비교와 정량화)

  • Cheong Cheong-jo;Choi Doo-hyoung;Kim Tae-keun;Okada Mitsumasa
    • Journal of the Korean Society for Marine Environment & Energy
    • /
    • v.4 no.4
    • /
    • pp.3-11
    • /
    • 2001
  • To know the seawater infiltration into tidal flat sediment in coastal area is very important, because it is significantly correlated with the infiltration and transportation of pollutants in soil, the supply of dissolved oxygen, nutrients and organic matter to benthic organisms for survival of benthic organisms and the seawater purification. So, we set up purpose to clarify the infiltration behavior of seawater by wave action in tidal flat, to clear the effects of slope of tidal flat and breaking wave height on seawater infiltration and to quantify the infiltration volume of seawater. For purpose, the seawater infiltration was studied with visualization method by using coloring tracer and transparent glass beads replaced as natural sediment in model tidal flat. Specific conclusions derived from this study are as follows. The semi-circular type infiltration of seawater by wave action into saturated sediment was a new infiltration behavior that was not considered in previous studies. The infiltration rate of seawater was increased with increasing of breaking wave height and slope of tidal flat. However, the effects of the slope was bigger than that of breaking wave height on seawater infiltration into tidal flat sediments. It was possible to calculate the infiltration volume of seawater by wave action in natural tidal flat sediment and in fields. Therefore, we can point out that wave action play an important role in the supply of dissolved oxygen, nutrients and organic matter to benthic organisms, transportation or diffusion of pollutants and seawater purification. So, we hope to be studied the supply of food to benthic organism, pollutant transport and seawater purification on the base of these results.

  • PDF

A study on the residues of fluoroquinolones in hen's eggs consumed in Incheon Metropolitan city (인천광역시에서 유통되는 계란의 플루오로퀴놀론계 항균물질 잔류 실태 조사)

  • Park, Eun-Jeong;Lim, Ji-Huen;Lee, Sung-Mo;Im, Jeong-Soo;Oh, Dae-Kyu
    • Korean Journal of Veterinary Service
    • /
    • v.31 no.3
    • /
    • pp.385-395
    • /
    • 2008
  • This study was carried out to investigate the residue level of fluoroquinolones in hen's general eggs and specific eggs by microbiological assay method and high performance liquid chromatography (HPLC) method. HPLC separation was carried out by reversed phase chromatography on a Symmetry $C_{18}$ (250${\times}$4.6 mm, $5{\mu}m$ particle size) with a phase composed of distilled water (containing 0.4% triethylamine and phosphoric acid) : Methanol (780 : 220, v/v), pumped isocratically at a flow rate of 1.0ml/min. A fluorescence detector was utilized with an excitation wavelength of 278nm and an emission wavelength of 456nm. The calibration curves were linear $({\gamma}^2{\geq}0.999)$ over a concentration range of $0.025{\sim}0.4{\mu}g/ml$. Average recoveries of the five fluoroquinolones in whole eggs at fortified levels of $0.05{\sim}0.2{\mu}g/g$ were ranged mean $78.1{\sim}91.7%$ and low coefficient of variation was less than 10% for all analysed samples. The limits of detection and limits of quantification for whole eggs were $1.2{\sim}6.0ng/g$ and $2.3{\sim}9.1ng/g$, respectively. Only one hen's general eggfrom chicken farm in Incheon was detected with the residual fluoroquinolones (Microbiological assay method; 1 of 47 general eggs) ; the range of residual concentration enrofloxacin was 0.12ppm. Those in food stores were detected with the residual fluoroquinolones (Microbiological assay method; 4 of 88 general eggs) ; the ranges of residual concentration enrofloxacin were $0.15{\sim}2.2 ppm$, ciprofloxacin $0.01{\sim}0.06ppm$, and hen's specific eggs (40) in food stores were not detected. For the microbiological assay method of fluoroquinolones in hen's eggs, as the results of comparative analysis, the disc diffusion method with E coli may be a little highly detected for the residual fluoroquinolones.

Endothelial Cell Proliferation and Vascular Endothelial Growth Factor Expression in Primary Colorectal Cancer and Corresponding Liver Metastases

  • Raluca, Balica Amalia;Cimpean, Anca Maria;Cioca, Andreea;Cretu, Octavian;Mederle, Ovidiu;Ciolofan, Alexandru;Gaje, Pusa;Raica, Marius
    • Asian Pacific Journal of Cancer Prevention
    • /
    • v.16 no.11
    • /
    • pp.4549-4553
    • /
    • 2015
  • Background: Colorectal carcinoma (CRC) is one of the major causes of cancer death worldwide. Data from the literature indicate differences between the proliferation rate of endothelial cells relative to the morphology growth type, possibly due to origin of specimens (autopsy material, surgery fragments) or quantification methods. Vascular endothelial growth factor (VEGF) is a factor that stimulates the proliferation of endothelial cells. It is expressed in more than 90% of cases of metastatic CRC. Aim: The aim of this study was to evaluate the endothelial cell proliferation and VEGF expression in primary tumors and corresponding liver metastases. Materials and Methods: Our study included 24 recent biopsies of primary tumors and corresponding liver metastases of CRC cases. CD34/Ki67 double immunostaining and RNA scope assay for VEGF were performed. Results: In the primary tumors analysis of VEGFmRNA expression indicated no significant correlation with differentiation grade, proliferative and non-proliferative vessels in the intratumoral and peritumoral areas. In contrast, in the corresponding liver metastases, VEGFmRNA expression significantly correlated with the total number of non-proliferative vessels and total number of vessels. CD34/Ki67 double immunostaining in the cases with poorly differentiated carcinoma indicated a high number of proliferating endothelial cells in the peritumoral area and a low number in the intratumoral area for the primary tumor. Moderately differentiated carcinomas of colon showed no proliferating endothelial cells in the intratumoral area in half of the cases included in the study, for both, primary tumor and liver metastasis. In well differentiated CRCs, in primary tumors, a high proliferation rate of endothelial cells in the intratumoral area and a lower proliferation rate in the peritumoral area were found. A low value was found in corresponding liver metastasis. Conclusions: The absence of proliferative endothelial cells in half of the cases for the primary tumors and liver metastases in moderately differentiated carcinoma suggest a vascular mimicry phenomenon. The mismatch between the total number of vessels and endothelial proliferation in primary tumors indicate that a functional vascular network is already formed or the existence of some mechanisms influenced by other angiogenic factors.

Development of Construction Project Performance Management System(PPMS) Considering Project Characteristics (건설 프로젝트 리스크 관리 효율성 향상을 위한 성과측정시스템(PPMS) 개발)

  • Cha, Hee-Sung;Kim, Ki-Hyun
    • Korean Journal of Construction Engineering and Management
    • /
    • v.14 no.1
    • /
    • pp.82-90
    • /
    • 2013
  • In the construction industry, there are so many qualitative factors affecting the performance of a project. So it is crucial to measure the factors in an effective way in order to analyze the interrelationship among the various factors. To improve the performance level of a project, it is also important to identify the most appropriate management practices which are inter-linked with the subject project. The purpose of this study is to develop a project performance management system (PPMS) to quantitatively analyze the variety of project performance data and identify the best management practice to increase the potential level of a particular performance area. Using a comparative statistical method, this study developed a quantification method and web-based computerized system to enhance the usage of the system. The system, however, is still under the validation stage because of the shortage of data set. In the future, when more and more completed project data are stored in the system, the system would play a crucial role in predicting the performance level and matching the best management practice for a subject project. In addition, the system can also be modified as a tool for a business- or industry-level system by incorporating the existing enterprise resource programs.