• Title/Summary/Keyword: Quantitation

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Quantitation of abamectin by HPTLC and its pharmacokinetics after intramuscular injection in pigs (돼지에서 근육주사한 Abamectin에 대한 HPTLC 분석 및 약물동태학)

  • Park, Seung-chun;Yun, Hyo-in
    • Korean Journal of Veterinary Research
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    • v.40 no.1
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    • pp.35-41
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    • 2000
  • We established a new method to analyze abamectin using HPTLC (high performance thin layer chromatography) in order to obtain its pharmacokinetic profiles in pigs. Recovery of abamectin in pig serum after fluorescence derivatization was $80.01{\pm}3.82%$ at 0.1ppm and $83.67{\pm}3.63%$ at 10ppm, respectively. Detection reproducibility in terms of coefficient variation (c.v.) was 3.09% and 2.74% (intra-day), and 3.71% and 51.7%(inter-day), for 0.1 and 10ppm, respectively. Pharmacokinetics of abamectin was studied in five Yorkshire-Landrace mixed bred male pigs ($35.0{\pm}2.7kg$) administered intramuscularly 0.3mg/kg b.w. Pharmacokinetic profiles of abamectin in pigs were described by the 1-compartment open model with first-order absorption and first-order elimination. AUC (area under the curve) was $262.65{\pm}16.44ng{\cdot}day/ml$ and the biological elimination half-life ($t_{1/2},\;k_e$) was $5.28{\pm}0.84$ days, indicating somewhat high bioavailability and long half-life by the intramuscular route. We suggest intramucular injection of abamectin could be also used in place of the recommended route of its subcutaneous administration so far.

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Microbial Risk Assessment (미생물학적 위해성 평가)

  • 이건형
    • Korean Journal of Microbiology
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    • v.37 no.2
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    • pp.101-108
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    • 2001
  • Risk assessment defines as the process of estimating both the probability that an event will occur and the probable magnitude of its adverse effects. Chemical or microbial risk assessment generally follows four basic steps, that is, hazard identification, exposure assessment, dose-response assessment, and risk characterization. Risk assessment provides an effective framework for determining the relative urgency of problems and the allocation of resources to reduce risks. Using the results of risk analyses, we can target prevention, reme-diation, or control effects towards areas, sources, or situations in which the greatest risk reductions can be achieved with resources available. Risk assessment is also used to explain chemical and microbial risks as well as ecosystem impacts. Moreover, this process, which allows the quantitation and comparison of diverse risks, lets risk managers utilize the maximum amount of complex information in the decision-making process. This information can also be used to weigh the cost and benefits of control options and to develop standards or treatment options.

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Dynamic MRM Measurements of Multi-Biomarker Proteins by Triple-Quadrupole Mass Spectrometry with Nanoflow HPLC-Microfluidics Chip

  • Ji, Eun-Sun;Cheon, Mi-Hee;Lee, Ju-Yeon;Yoo, Jong-Shin;Jung, Hyun-Jin;Kim, Jin-Young
    • Mass Spectrometry Letters
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    • v.1 no.1
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    • pp.21-24
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    • 2010
  • The development of clinical biomarkers involves discovery, verification, and validation. Recently, multiple reaction monitoring (MRM) coupled with stable isotope dilution mass spectrometry (IDMS) has shown considerable promise for the direct quantification of proteins in clinical samples. In particular, multiple biomarkers have been tracked in a single experiment using MRM-based MS approaches combined with liquid chromatography. We report here a highly reproducible, quantitative, and dynamic MRM system for validating multi-biomarker proteins using Nanoflow HPLC-Microfluidics Chip/Triple-Quadrupole MS. In this system, transitions were acquired only during the retention window of each eluting peptide. Transitions with the highest MRM-MS intensities for the five target peptides from colon cancer biomarker candidates were automatically selected using Optimizer software. Relative to the corresponding non-dynamic system, the dynamic MRM provided significantly improved coefficients of variation in experiments with large numbers of transitions. Linear responses were obtained with concentrations ranging from fmol to pmol for five target peptides.

An HPLC method for the determination of thioctic acid in raw material and tablets

  • Mai, Xuan-Lan;Ahn, GyeChan;Lee, SeokHan;Kang, Jong-Seong;Woo, Mi Hee;Na, Dong-Hee;Chun, In-Koo;Kim, Kyeong Ho
    • Analytical Science and Technology
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    • v.30 no.5
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    • pp.221-225
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    • 2017
  • Thioctic acid is a vitamin-like antioxidant which is prepared as tablets and injection. The Korean Pharmacopoeia (KP XI) contains monograph for the quality control of raw thioctic acid using ultra-violet visible spectrophotometry and its formulations using high performance liquid chromatography (HPLC). In British Pharmacopoeia 2013 (BP2013), another HPLC method is used for the assay test of thioctic acid material. For the international harmonization, we present an HPLC method for quantitation of thioctic acid in both raw material and tablets. Method validation was performed to determine linearity, precision, accuracy, system suitability, and robustness. The linearity of calibration curves in the desired concentration range was high ($r^2=0.9995$), while the RSDs for intra- and inter-day precision were 0.93 ~ 1.26 % and 1.40 ~ 1.76 %, respectively. Accuracies ranged from 98.13-100.00 %. Since the system suitability, intermediate-precision and robustness of the assay were satisfactory, this method will be a valuable addition to the Korean Pharmacopoeia (KP XI).

Synthesis of Hapten for Indirect Competitive Immunoassay for Measuring 3,5,6-trichloro-2-pyridinol

  • Kim, Areumnuri;Kim, Joong-Young;Jeong, Sang-Hee;Cho, Myung-Haing;Park, Kyung-Hun;Cho, Namjun;Paik, Min Kyoung
    • Korean Journal of Environmental Agriculture
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    • v.34 no.4
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    • pp.345-349
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    • 2015
  • BACKGROUND: In this study, we have attempted to identify a urinary biomarker to assess chlorpyrifos exposure in farmers. The major metabolite and the excretion pathway of chlorpyrifos is 3,5,6-trichloro-2-pyridinol (TCP) in urine. Herein, we describe an adequate synthetic method for TCP hapten for measuring urinary TCP of farmers. METHODS AND RESULTS: First, TCP was prepared by spacer attachment through hydrolysis of thiophosphate ester from chlorpyrifos. After reaction with benzyl bromide, the TCP was transformed into 2,3,5-trichloro-6-benzyloxypyridine. Next, the chlorine in the 2 nd position of the pyridyl ring was substituted into 3-mercaptopropanoic acid spacer arm. Finally, the phenyl group attached to the 6 th position in pyridyl ring was removed for producing the targeted product, 3-(3,5-Dichloro-6-hydroxy-2-pyridyl) thiopropanoic acid. CONCLUSION: Henceforth, this TCP hapten would be used in developing immunoassay studies for the detection and quantitation of urinary TCP of farmers.

Developing a Web-based System for Computing Pre-Harvest Residue Limits (PHRLs)

  • Chang, Han Sub;Bae, Hey Ree;Son, Young Bae;Song, In Ho;Lee, Cheol Ho;Choi, Nam Geun;Cho, Kyoung Kyu;Lee, Young Gu
    • Agribusiness and Information Management
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    • v.3 no.1
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    • pp.11-22
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    • 2011
  • This study describes the development of a web-based system that collects all data generated in the research conducted to set pre-harvest residue limits (PHRLs) for agricultural product safety control. These data, including concentrations of pesticide residues, limit of detection, limit of quantitation, recoveries, weather charts, and growth rates, are incorporated into a database, a regression analysis of the data is performed using statistical techniques, and the PHRL for an agricultural product is automatically computed. The development and establishment of this system increased the efficiency and improved the reliability of the research in this area by standardizing the data and maintaining its accuracy without temporal or spatial limitations. The system permits automatic computation of the PHRL and a quick review of the goodness of fit of the regression model. By building and analyzing a database, it also allows data accumulated over the last 10 years to be utilized.

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GC/MS and GC/ECD Analysis of Residual Pesticides in Herbal drugs (GC/MS와 GC/ECD를 이용한 한약재 중 잔류 농약의 분석)

  • Kim, Ho-Kyoung;Park, So-Yeon;Ko, Byoung-Seob
    • The Journal of Korean Medicine
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    • v.20 no.1 s.37
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    • pp.44-51
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    • 1999
  • Analysis of residual pesticides in herbal drugs was performed by GC-ECD and GC-MS. Especially, selected ion monitoring(SIM) technique was applied to increase the GC/MS sensitivity. Analysis of residual pesticides was determined sensitivity and selectively without any internal standard by setting the SIM technique to their characteristic fragments for quantitation ion and confirmation ion. The combination of two detector, GC-ECD and MS-SIM technique, is abailable for determining a multiclass residual pesticides in herbal drugs. The average recoveries through the method were $65.9%{\sim}99.7%$ in herbal drugs. The data of gas chromatographic analysis was compared with the limits of residual pesticides in herbal drugs and agricultural foods. 4. 4-DDT was detected above the limits to the residual pesticides in herbal drugs. Diazinon and EPN were detected, but the limits of residual pesticides were less than that of agricultural foods.

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Simultaneous Determination of Amphetamine-Type Stimulants (ATS) in Human Hair by GC-MS (가스크로마토그래피-질량분석기를 이용한 모발에서 암페타민형 각성제 약물의 동시 분석)

  • 김진영;서승일;고범준;이재일;정재철;서용준;인문교
    • YAKHAK HOEJI
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    • v.47 no.3
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    • pp.142-147
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    • 2003
  • Gas chromatography-mass spectrometric (GC-MS) procedure is presented for the simultaneous qualification and quantitation of methamphetamine (MA), amphetamine (AMP), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA), and 3,4-methylenedioxyethylamphetamine (MDEA) in human hair. The method procedure involves decontamination of hair with distilled water and acetone, acidic hydrolysis, extraction in the presence of deuterated internal standards, and GC-MS analysis after derivatization with trifluoroacetic anhydride (TFAA) in ethylacetate. The limit of detection for 5 drugs were about 0.1∼0.15 ng/mg using 30 mg hair sample. Coefficient variations of correlation ranged from 0.9941 to 0.9993. The recoveries of these drugs were found to be 93.4∼104.4%. The concentrations of AMP, MA, MDA, and MDMA in abusers' hair samples were measured 0.17∼2.88, 2.09∼18.34, 0.24∼3.83, and 3.10∼22.81 ng/mg, respectively. The ratios of MA/AMP and MDMA/MDA ranged 5.67∼49.57 and 4.78∼54.31, respectively. This assay has been successfully utilized in the evaluation of the deposition of amphetamine-type stimulants (ATS) in human hair.

Quantitation of Recombinant Hirudin by Enzyme-Linked Immunosorbent Assay (효소면역측정법 (ELISA)을 이용한 유전자 재조합 히루딘의 정량)

  • Choi, Yun-Joo;Hahn, Bum-Soo;Ahn, Mi-Young;Park, Pyung-Keun;Sohn, Jung-Hoon;Choi, Eui-Sung;Lee, Sang-Ki;Kim, Yeong-Shik
    • YAKHAK HOEJI
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    • v.41 no.1
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    • pp.74-80
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    • 1997
  • A polygonal antibody against recombinant hirudin was raised for the development of a ELISA in biological fluids. Recombinant hirudin was conjugated to maleimide activated carrie r protein, KLH and injected to a rabbit. The third booster collection of antiserum was used as primary antibody for the ELISA. The titer for the detection antibody was determined. The direct ELISA could determine the concentration of hirudin in the range of ~10ng/ml. Affinity pulified IgG was obtained and conjugated to horseradish peroxidase. Purified IgG and IgG-HRP could be used as capture and detection antibody, respectively. Although sandwich ELISA would not give the satisfactory results. it could apply for the detection of hirudin level in the range of ~20 ${\mu}$g/ml.

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Determination of Free Amino Acids in Isatidis Radix By HILIC-UPLC-MS/MS

  • Pan, Yilin;Li, Jin;Li, Xiang;Chen, Jianwei;Bai, Ganggang
    • Bulletin of the Korean Chemical Society
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    • v.35 no.1
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    • pp.197-203
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    • 2014
  • A rapid, accurate and precise method for the determination of 22 amino acids in Isatidis Radix by Hydrophilic Interaction Ultra-High-Performance Liquid Chromatography Coupled with Triple-Quadrupole Mass Spectrometry (HILIC-UPLC-MS/MS) was established. Chromatographic separation was carried out on a Acquity UPLC BEH Amide column ($2.1mm{\times}100mm$, $1.7{\mu}m$) with gradient elution of acetonitrile (containing 0.05% formic acid and 2 mM ammonium formate) and water (containing 0.15% formic acid and 10 mM ammonium formate) at a flow rate of 0.4 mL/min; Waters Xevo$^{TM}$ TQ worked in multiple reaction monitoring mode. All components were separated in 17 min. All calibration curves were linear ($R^2$ > 0.991) over the tested ranges. The limits of detection (LOD) and limits of quantitation (LOQ) for these compounds were 0.21-79.55 and 0.72-294.23 ng/mL, respectively. The average recoveries were in the range of 93.75-104.16% with RSD value less than 6.56%. Therefore, this method could be an alternative assay for the determination of 22 amino acids in Isatidis Radix due to its rapidness, sensitivity, less sample and solvent consumption.