• Title/Summary/Keyword: Quantification I method

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The Use of qNMR for Quality Control of Coumarin-based Pharmaceuticals and Plant Medicines

  • Crocoli, Luana C.;Molon, Vinicius B.;Moura, Sidnei
    • Natural Product Sciences
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    • v.27 no.2
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    • pp.128-133
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    • 2021
  • The Coumarin (1,2-benzopyrone) is the main secondary metabolite of Mikania laevigata Sch. Beep ex Baker and Mikania glomerata Spreng., which are popularly known as guaco. These plants have been used mainly in traditional medicine in the treatment of respiratory diseases because their bronchodilator effect. However, there are around 200 species of Mikania, which are quite similar in appearance. From these, only M. leavigata and M. glomerata have high concentrations of coumarins. In this line, the falsification of products Mikania based has been frequent. In this sense, this work demonstrated the application of the easy, fast, e not destructive method based in Nuclear Magnetic Resonance in quantitative mode (qNMR) for the determination of coumarin in both commercial and homemade guaco products. Thus, in the first step the compounds were extract from guaco leaves and syrups using chloroform (CHCl3), with or without ultrasound. About the method, was linear with a R2 = 0.9947 for 1,2-benzopyrone, with detection and quantification limits with were 0.11 and 0.36 mg mL-1 respectively. In the same line, the method was safe with RSD <0.3% and with recovery ranging from 93-101%. To confirm the applicability of the method, in the last step was applied to 10 real samples (6 from leaves and 4 from syrups). The content of the coumarin in the leaf extract ranged from 0.62 to 1.30 mg mL-1. For syrups I, II and IV, the content of coumarin was in accordance with the manufacturers. However, for de Syrup III, the concentration was 155% higher. In summary, the qNMR is a rapid method with minimal sample preparation that can be used to quantify coumarin in home-made plant extracts as well as in commercial samples as syrup for instance. This method is applicable for quality control of different plants-based products.

Estimation of Growing Stock and Carbon Stock based on Components of Forest Type Map: The case of Kangwon Province (임상도 특성에 따른 임목축적 및 탄소저장량 추정: 강원도를 중심으로)

  • Kim, So Won;Son, Yeong Mo;Kim, Eun Sook;Park, Hyun
    • Journal of Korean Society of Forest Science
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    • v.103 no.3
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    • pp.446-452
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    • 2014
  • This research aimed to provide a method to estimate growing stock and carbon stock using the characteristics of forest type map such as the age-class, DBH class and crown density class. We transformed the growing stock data of national forest inventory (mainly Kangwon-do province) onto those of time when the forest type map was established. We developed a simulation model for the growing stock using the transformed data and the characteristics of forest type map by the quantification method I. By comparing partial correlation coefficient, we found that quantification of growing stock was largely affected by age-class followed by crown density class, forest type and DBH class. The growing stock, was estimated as minimum in the broadleaved forest with age-class II, DBH class 'Small', and crown density class 'Low' as $20.0m^3/ha$, whereas showed maximum value in the coniferous forest with age-class VI, DBH class 'Large', and crown density class 'High' as $305.0m^3/ha$. The growing stock for coniferous, broadleaved, and mixed forest were estimated as $30.5{\sim}305.0m^3/ha$, $20.0{\sim}200.4m^3/ha$, and $23.8{\sim}238.1m^3/ha$, respectively. When we compared the carbon stock by forest type, the carbon stock by age class based on growing stock was maximum when DBH class was 'Large' and crown density class was 'High' regardless of forest type. This estimation of growing stock by using characteristic of forest type can be used to estimate the changes in growing stock and carbon stock resulting from deforestation or natural disaster. In addition, we hope it provide a useful advice when forest officials and policy makers have to make decisions in regard to forest management.

Simultaneous Determination of Five Porphyrins in Human Urine and Plasma Using High Performance Liquid Chromatography-Tandem Mass Spectrometry

  • Hur, Yeoun;Tae, Sookil;Koh, Yun-Joo;Hong, Sung-Hyun;Yoon, Young Ho;Jang, Haejong;Kim, Sooji;Kim, Kyeong Ho;Kang, Seung Woo;Lee, Youngshin;Han, Sang Beom
    • Mass Spectrometry Letters
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    • v.5 no.2
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    • pp.42-48
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    • 2014
  • A specific and sensitive liquid chromatography-electrospray ionization tandem mass spectrometry method (LC-ESI-MS/MS) was developed and validated for the simultaneous quantification of porphyrins (coproporphyrin, pentacarboxylporphyrin, hexacarboxylporphyrin, heptacarboxylporphyrin, and uroporphyrin) in human plasma and urine. Acidified plasma samples and urine samples were prepared by using liquid-liquid extraction using ethyl acetate and protein precipitation with acetonitrile, respectively. The separation was achieved onto a Synergi Fusion RP column ($150mm{\times}2.0mm$, $4{\mu}m$) with a gradient elution of mobile phase A (0.1% formic acid in 2 mmol/L ammonium acetate, v/v) and mobile phase B (20% methanol in acetonitrile, v/v) at a flow rate of $450{\mu}L$/min. Porphyrins and the internal standard (IS), coproporphyrin I-$^{15}N_4$, were detected by a tandem mass spectrometer equipped with an electrospray ion source operating in positive ion mode. Multiple reaction monitoring (MRM) transitions of the protonated precursor ions and the related product ions were optimized to increase selectivity and sensitivity. The proposed method was validated by assessing selectivity, linearity, limit of quantification (LOQ), precision, accuracy, recovery, and stability. The calibration curves were obtained in the range of 0.1-100 nmol/L and the LOQs were estimated as 0.1 nmol/L for all porphyrins. Results obtained from the validation study of porphyrins showed good accuracy, precision, recovery, and stability. Finally, the proposed method was successfully applied to clinical studies on the autism spectrum disorder (ASD) diagnosis of 203 Korean children.

Development of Assessment Model for the Optimal Site Prediction of Evergreen Broad-leaved Trees in Warm Temperate Zone according to Climate Change (기후변화에 따른 난대상록활엽수의 적지예측 평가 모델 개발)

  • Kang, Jin-Teak;Kim, Jeong-Woon;Kim, Cheol-Min
    • Journal of agriculture & life science
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    • v.46 no.3
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    • pp.47-58
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    • 2012
  • This study was carried out to develop assessment model for the optimal site prediction of Dendropanax morbifera, Evergreen broad-leaved trees in warm temperate zone according to climate change. It was created criterion for assessment model of the optimal site prediction by quantification method to possible analysis of quantitative and qualitative data, through study relationship between growth of tree and site environmental factors. A program of the optimal site prediction was developed using program version 3.2, an Avenue and Dialog Designer tool of ESRI as GIS(geographic information system) engine. Developed program applied to test accuracy of the optimal site prediction in study area of Wando, Jeollanam-do, having a various evergreen broad-leaved trees of warm temperate zone. In the results from analysis of the optimal site prediction on Dendropanax morbifera, the characteristics of optimal site were analyzed site environmental features with 401~500m of altitude, $15^{\circ}$ of slope, hillside of local topography, alluvium of deposit type, convex of slope type and south of aspect. The mapping area per grade of the optimal site prediction in the Dendropanax morbifera showed 1,487.2ha(25.4%) of class I, 1,020.3ha(17.4%) of class II, 2,231.8ha(38.2%) of class III and 1,110.5ha(19.0%) of class IV.

Simultaneous Quantification of Sulfonamide and Tetracyclines in Fish Muscle Tissue by Matrix Solid Phase Dispersion (MSPD) Extraction and HPLC (MSPD와 HPLC를 이용한 어류의 잔류 설파제와 테트라사이클린계 항생물질의 동시분석)

  • 하대식;김종수;김곤섭
    • Journal of Food Hygiene and Safety
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    • v.12 no.2
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    • pp.117-124
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    • 1997
  • A simple, rapid and simultaneous analytical method is described for the detection of Sulfonamide and Tetracycline residues, i.e., Sulfamerazine (SMR), Sulfamethazine (SMT), Sulfamonomethoxine (SMM), Sulfadimethoxine (SDM), Sulfaquinoxaline (SQN), Oxytetracycline (OXY), Tetracycline (TC), Chlortetracycline (CTC). Blank control and sulfonamide and tetracycline fortified fish muscle samples (0.5 f) were blended with octadecylsilyl (C18, 40 ${\mu}{\textrm}{m}$, 21% load, 60$\AA$) derivatized silica packing material (2 g). Blended fish samples were washed with hexane, then, benzene and dichloromethace were used for the elution of tetracycline and sulfonamide were analyzed by HPLC. Correlation coefficients of standard curves for individual sulfonamide and tetracycline isolated from fortified samples were linear (0.9993$\pm$0.0003~0.9997$\pm$0.0003, 0.9493$\pm$0.078~0.9753$\pm$0.036), respectively. The average percentage recoveries of sulfonamide and tetracycline ranged as 80.86~96.52% to 85.88~92.23%, and 30.01~37.12% to 65.89~73.40%, for the concentration range (0.1~1.0 ppm) examined, respectively. Limit of detection for sulfonamide was 0.0012 ppm for SMR in Paralichthys Olivacleus and 0.0020 ppm for SMR, 0.015 ppm for SMM in Cyprinus Carpio. The applicability of this procedure is demonstrated by separation and detection of incurred tetracycline and sulfonamide residues in fish muscle tissue.

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The influence of residual stress on the engineering behaviour of rock (잔류응력이 암석의 공학적 거동에 끼치는 영향)

  • 박형동
    • Tunnel and Underground Space
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    • v.5 no.4
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    • pp.363-375
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    • 1995
  • Critical literature review in this study revealed that there can be a significant influence of the residual stress on the engineering properties of rock. The review also showed that few number of research works on the quantification of the influence was attributed to the limitation of the two classical measurement techniques, viz, X-ray diffraction and mechanical relaxation method. In this study, a new way of approach was sought based on the assumption that residual stress up to the failure. A series of hoop tests conducted onthe samples from the limb of Carboniferous Limestone in Clevedon, England, revealed that (i) there is no preferential orientations of microcracks and minerals which have been widely believed as the main source of the strength anisotropy of rock; (ii) the anisotropy of the tensile strength of the limestone results from the influence of the residual stress; (iii) since jointing commenced within the fold, residual stored strain energy has been released preferentially in the direction perpendicular to the major joints(o$^{\circ}$ and 90$^{\circ}$); (ⅳ) during the hoop test making it much easier to create tensile fracture in these directons, viz 45$^{\circ}$ and 135$^{\circ}$)was released during the hoop test making it much easier to create tensile fracture in these directions, viz 45$^{\circ}$and 135$^{\circ}$;(v) the direction in which the stored strain energy may be presumed to be the least, required the greatest work to cause failure.

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A Study on the Quantification of Qualitative Attributes in Industrial Design (질적 디자인 가치의 수량화(I))

  • 우흥룡
    • Archives of design research
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    • v.2 no.1
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    • pp.117-130
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    • 1989
  • Evaluation is to be seen a~ a central component of design activity. It is an attempt to ensure that the proposal which arises is accepted and that the resulting artefact itself suited to its purposes in practice. Recent surveys of Evaluation show that most methods require quantitative and explicit attributes. Always a significant part of the attributes of design proposals is qualitative. Therefore we need some study that convert qualitative attributes into quantitative scale values, because in many cases con\ulcornerclusions can be drawn about the order of the overall value of the design proposals. Following to Thurstone's psychological scaling methods, attributive values are assigned by ruting scale methods, met, hod of rank-order and method of paired comparisons. The problem of psycho\ulcornerlogical scaling is then to determine whether the stimuli can be ordered on a psychological continuum with respect to the degree of the attributes each possesses. The law of comparative judgement assumes that for a given stimulus there is associated a most frequently aroused or modal discriminal process on a psychological continuum. This paper is based upon the premise that the modal discriminul process will also be the same as the mean or median of the distribution.The objective of this paper is to argue for an acceptance of qualitative approaches to the evalua\ulcornertion of Design as a complement to the existing quantitative techniques. The scale values of 10 attri\ulcornerbutes \ulcorner(1) originality, (2) aesthetics, (3) satisfaction, (4) effeciency, (5) function, (6) size, (7) texture, (8) simplicity, (9) symbol, and (10) facility) in case of TV sets are obtained and their interactions are examined.

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Quantitative Assay of Recombinant Hepatitis B Surface Antigen by Using Surface Plasmon Resonance Biosensor (Surface plasmon resonance 바이오센서를 이용한 재조합 B형 간염 표면항원의 정량분석)

  • Lee, E. K.;Ahn, S. J.;Yoo, C. H.;Ryu, K.;Jeon, J. Y.;Lee, H. I.;Choi, S. C.;Lee, Y. S.
    • KSBB Journal
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    • v.17 no.1
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    • pp.20-25
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    • 2002
  • We performed a basic experiment for rapid, on-line, real-time measurement of HBsAg by using a surface plasmon resonance biosensor to quantify the recognition and interaction of biomolecules. We immobilized the anti-HBsAg polyclonal antibody to the dextran layer on a CM5 chip surface which was pre-activated by N-hydroxysuccinimide for amine coupling. The binding of the HBsAg to the immobilized antibody was measured by the mass increase detected by the change in the SPR signal. The binding characteristics between HBsAg and its antibody followed typical monolayer adsorption isotherm. When the entire immobilized antibody was interacted, there was no additional, non-specific binding observed, which suggested the biointeraction was very specific as expected and independent of the ligand density. No significant steric hindrance was observed at 17.6 nm/$mm^2$ immobilization density. The relationship between the HBsAg concentration in the sample solution and the antigen bound to the chip surface was linear up to ca. $40\mu\textrm{g}$/mL, which is much wider than that of the ELISA method. It appeared the antigen-antibody binding was increased as the immobilized ligand density increased, but verification is warranted. This study showed the potential of this biosensor-based method as a rapid, simple, multi-sample, on-line assay. Once properly validated, it can serve as a more powerful method for HBsAg quantification replacing the current ELISA method.

Multiclass Method for the Determination of Anthelmintic and Antiprotozoal Drugs in Livestock Products by Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry

  • Hyunjin Park;Eunjung Kim;Tae Ho Lee;Sihyun Park;Jang-Duck Choi;Guiim Moon
    • Food Science of Animal Resources
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    • v.43 no.5
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    • pp.914-937
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    • 2023
  • The objective of this study was to establish a multi-residue quantitative method for the analysis of anthelmintic and antiprotozoal drugs in various livestock products (beef, pork, and chicken) using ultra-high-performance liquid chromatography-tandem mass spectrometry. Each compound performed validation at three different levels i.e., 0.5, 1, and 2× the maximum residue limit according to the CODEX guidelines (CAC/GL 71-2009). This study was conducted according to the modified quick, easy, cheap, effective, rugged, and safe procedure. The matrix-matched calibrations gave correlation coefficients >0.98, and the obtained recoveries were in the range of 60.2%-119.9%, with coefficients of variation ≤32.0%. Furthermore, the detection and quantification limits of the method were in the ranges of 0.03-3.2 and 0.1-9.7 ㎍/kg, respectively. Moreover, a survey of residual anthelmintic and antiprotozoal drugs was also carried out in 30 samples of beef, pork, and chicken collected in Korea. Toltrazuril sulfone was detected in all three samples. Thus, our results indicated that the developed method is suitable for determining the anthelmintic and antiprotozoal drug contents in livestock products.

Development of Analytical Method for the Determination and Identification of Unregistered Pesticides in Domestic for Orange and Brown Rice(I) -Chlorthal-dimethyl, Clomeprop, Diflufenican, Hexachlorobenzene, Picolinafen, Propyzamide- (식품공전 분석법 미설정 농약의 잔류분석법 확립(I) -Chlorthal-dimethyl, Clomeprop, Diflufenican, Hexachlorobenzene, Picolinafen, Propyzamide-)

  • Chang, Hee-Ra;Kang, Hae-Rim;Kim, Jong-Hwan;Do, Jung-A;Oh, Jae-Ho;Kwon, Ki-Sung;Im, Moo-Hyeog;Kim, Kyun
    • Korean Journal of Environmental Agriculture
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    • v.31 no.2
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    • pp.157-163
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    • 2012
  • BACKGROUND: For the safety of imported agricultural products, the study was conducted to develop the analytical method of unregistered pesticides in domestic. The analytical method of 6 pesticides, chlorthal-dimethyl, clomeprop, diflufenican, hexachlorobenzene, picolinafen, and propyzamide, for a fast multi-residue analysis were established for two different type crops, orange and brown rice by GC-ECD and confirmed by mass spectrometry. METHODS AND RESULTS: The analytical method was evaluated to limit of quantification, linearity and recoveries. The crop samples were extracted with acetonitrile and performed cleanup by liquid-liquid partition and Florisil SPE to remove co-extracted matrix. The extracted samples were analyzed by GC-ECD with good sensitivity and selectivity of the method. The limits of quantification (LOQ) range of the method with S/N ratio of 10 was 0.02~0.05 mg/kg for orange and brown rice. The linearity for targeted pesticides were $R^2$ >0.999 at the levels ranged from 0.05 to 10.0 mg/kg. The average recoveries ranged from 74.4% to 110.3% with the percentage of coefficient variation in the range 0.2~8.8% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in brown rice. And the average recoveries ranged from 77.8% to 118.4% with the percentage of coefficient variation in the range 0.2~6.6% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in orange. Final determination was by gas chromatography/mass spectrometry/selected ion monitoring (GC/MS/SIM) to identify the targeted pesticides. CONCLUSION: As a result, this developed analytical method can be used as an official method for imported agricultural products.