• Title/Summary/Keyword: Quantification Method

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Comparative Study of Extracting Fragrance Allergens by GC-MS/MS

  • Lee, In Ja;Ahn, Jae-Chan;Kim, Bogsoon;Chung, Deukmo
    • Mass Spectrometry Letters
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    • v.8 no.1
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    • pp.18-22
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    • 2017
  • Products containing any one or more of 26 fragrance allergens likely to cause contact allergies, are required under the 2008 domestic cosmetic law to be labeled when their concentrations exceed a certain range. This study focuses on the comparison and development of analytical methods based on headspace-solid phase micro extraction (HS-SPME) and liquid-liquid extraction (LLE) methods followed by GC-MS/MS for 24 of the fragrance allergens excepting for two natural materials in water samples. Using the developed HS-SPME method, 15 of the 24 fragrance allergens were analyzed and 9 compounds which have relatively low $logK_{OW}$ values (below about 2.5) were not extracted, and the correlation coefficient ($r^2$) of the calibration curve for quantification showed linearity of 0.9969 or more, and the method detection limits (MDL) and the limits of quantification (LOQ) were $0.078{\sim}0.582{\mu}g/L$ and $0.261{\sim}1.940{\mu}g/L$, respectively. In the case of using the optimized LLE method, all 24 fragrance allergens were analyzed, and the correlation coefficient ($r^2$) of the calibration curve for quantification showed linearity of 0.9957 or more, MDL and LOQ were $0.020{\sim}0.138{\mu}g/L$ and $0.065{\sim}0.440{\mu}g/L$, respectively.

Development of a Simultaneous Detection and Quantification Method of Anorectics in Human Urine Using GC-MS and its Application to Legal Cases (GC-MS를 이용한 사람 뇨시료 중 비만치료제 분석 및 비만치료제 남용 현황의 법과학적 고찰)

  • Choi, Hyeyoung;Lee, Jaesin;Jang, Moonhee;Yang, Wonkyung;Kim, Eunmi;Choi, Hwakyung
    • YAKHAK HOEJI
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    • v.57 no.6
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    • pp.420-425
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    • 2013
  • Phentermine (PT) and phenmetrazine (PM) have been widely used as anti-obesity drugs. These drugs should be used with caution due to its close relation to amphetamine in its structure and toxicity. PT and PM, amphetamine-type anorectics, have recently been considered as alternatives for methamphetamine abuse in Korea. In addition, the misuse and abuse of PT and PM obtained by illegal sources such as the internet become a serious social problem. In the present study, a simultaneous detection and quantification method for determining PT and PM in human urine was developed and validated according to the international guidelines. The urine samples were screened using a fluorescence polarization immunooassay and analyzed by gas chromatography mass spectrometry (GC-MS) after extraction using automatic solid phase extraction (SPE) with a mixed-mode cation exchange cartridge and derivatization with pentafluoropropionic anhydride (PFPA). The validation results for selectivity, linearity, limits of detection (LOD) and quantification (LOQ), intra- and inter-assay precision and accuracy and recovery were satisfactory. The validated method was successfully applied to authentic urine samples collected from 38 drug abuse suspects. PT and/or PM were identified with or without methamphetamine in urine samples. Abuse of PT and PM have increased continuously in Korea, therefore, closer supervision of the inappropriate use of anoretics is necessary.

A Simple Carbamidomethylation-Based Isotope Labeling Method for Quantitative Shotgun Proteomics

  • Oh, Donggeun;Lee, Sun Young;Kwon, Meehyang;Kim, Sook-Kyung;Moon, Myeong Hee;Kang, Dukjin
    • Mass Spectrometry Letters
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    • v.5 no.3
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    • pp.63-69
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    • 2014
  • In this study, we present a new isotope-coded carbamidomethylation (iCCM)-based quantitative proteomics, as a complementary strategy for conventional isotope labeling strategies, with providing the simplicity, ease of use, and robustness. In iCCM-based quantification, two proteome samples can be separately isotope-labeled by means of covalently reaction of all cysteinyl residues in proteins with iodoacetamide (IAA) and its isotope (IAA-$^{13}C_2$, $D_2$), denoted as CM and iCCM, respectively, leading to a mass shift of all cysteinyl residues to be + 4 Da. To evaluate iCCM-based isotope labeling in proteomic quantification, 6 protein standards (i.e., bovine serum albumin, serotransferrin, lysozyme, beta-lactoglobulin, beta-galactosidase, and alpha-lactalbumin) isotopically labeled with IAA and its isotope, mixed equally, and followed by proteolytic digestion. The resulting CM-/iCCM-labeled peptide mixtures were analyzed using a nLC-ESI-FT orbitrap-MS/MS. From our experimental results, we found that the efficiency of iCCM-based quantification is more superior to that of mTRAQ, as a conventional nonisobaric labeling method, in which both of a number of identified peptides from 6 protein standards and the less quantitative variations in the relative abundance ratios of heavy-/light-labeled corresponding peptide pairs. Finally, we applied the developed iCCM-based quantitative method to lung cancer serum proteome in order to evaluate the potential in biomarker discovery study.

Study on the Marker Steroids of New Zealand Deer (Cervus elaphus var. scoticus) Velvet Antler by UPLC-MS/MS and HPLC-PDA Methods - (II)

  • Lee, Nam Kyung;Jang, Kyoung Hwa;Lee, Jong Tae;Park, Hee Won;Han, Sung Tai;In, Gyo
    • Natural Product Sciences
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    • v.25 no.1
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    • pp.49-58
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    • 2019
  • Eleven steroid hormones (SHs: androstene-3,17-dione, estrone, ${\beta}$-estradiol, ${\alpha}$-estradiol, testosterone, dehydroepiandrosterone, $17{\acute{a}}$-hydroxyprogesterone, medroxyprogesterone, megestrol acetate, progesterone, and androsterone) were detected from New Zealand deer (Cervus elaphus var. scoticus) velvet antler (NZA, 鹿茸 ). A method for the quantification of eleven SHs was established by using ultraperformance liquid chromatography (UPLC)-MS/MS. The linearities ($R^2$ > 0.991), limits of quantification (LOQ values, 0.3 ng/mL to 23.1 ng/mL), intraday and interday precisions (relative standard deviation: RSD < 2.43%), and recovery rates (97.3% to 104.6%) for all eleven SHs were determined. In addition, a method for the quantification of three 7-oxycholesterols (7-O-CSs: 7-ketocholesterol, $7{\alpha}$-hydroxycholesterol, and $7{\beta}$-hydroxycholesterol) in the NZA was established by using an HPLC-photodiode array (PDA) method. The linearities ($R^2$ > 0.999), LOQ values (30 ng/mL to 350 ng/mL), intraday and interday precisions (RSD < 1.93%), and recovery rates (97.2% to 103.5%) for the three 7-O-CSs were determined. These quantitative methods are accurate, precise, and reproducible. As a result, it is suggested that the five steroid compounds of androstene-3,17-dione, androsterone, 7-ketocholesterol, $7{\alpha}$-hydroxycholesterol, and $7{\beta}$-hydroxycholesterol could be marker steroids of NZA. These methods can be applied to quantify or standardize the marker steroids present in NZA.

Quantification of Ecological Impact as a Basis for Evaluation (독일에서의 환경영향의 정량적 평가)

  • Schweppe-Kraft, Burkhard
    • Journal of Environmental Impact Assessment
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    • v.2 no.2
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    • pp.59-71
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    • 1993
  • Evaluation methods are employed in environmental impact assessment to choose between different project site, to determine the required measures to compensate impact and to decide whether the environmental impacts are more important than the social or economic effects of a project. The main obstacles that restrict use of quantitative evaluation method are a Lack of knowledge about the environmental effects (e.g. if impacts on wildlife or landscape amenities are predicted) and the relative importance of economic and social issues compared with nature conservation stability of ecosystem or landscape beauty. In Germany, the most common method for site planning is the "ecological risk analysis". It is a kind of multi-criteria-decision-method based on quantitative and qualitative description and ordinal ranking. The various kinds of "ecological balancing methods" that are more recently developed (within the last decade) to quantify the required amount for compensatory measures instead often use cardinal figures to express the value of ecosystems, the intensity of impacts, the need for additional measures to compensate for long recuperative periods when restoring ecosystems and so on. There are still only a view attempts to quantify decisions between environmental and socio-economic issues. Multicriteria-analysis as well as cost-benifit-analysis was used. Some new approaches which are still in a preliminary status are based on contingent valuation and on calculations for compensatory payments (instead of compensatory measures).

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Simultaneous Determination of Platyphylloside, Aceroside VIII and Betulin in Betula platyphylla bark by HPLC-DAD (HPLC-DAD를 이용한 자작나무 수피의 Platyphylloside, Aceroside VIII 및 Betulin의 동시분석법 확립)

  • Cho, NamKi;Kim, Dae Hyun;Sung, Sang Hyun
    • Korean Journal of Pharmacognosy
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    • v.45 no.4
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    • pp.294-299
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    • 2014
  • The simultaneous determination of platyphylloside, aceroside and betulin was established for the quality control of Betula platyphylla bark using a high performance liquid chromatography and diode-array UV/Vis detector (HPLC-DAD). Separation and quantification were successfully achieved with a INNO C18 column ($5{\mu}m$, 4.6 mm $I.D.{\times}150mm$) by gradient elution of a mixture of methanol and water at a flow rate of 1.0 ml/min. Validation of the developed method was performed by various factor such as linearity, specificity, precision, accuracy, system suitability and stability. This method was successfully applied to the determination of contents of platyphylloside, aceroside VIII and betulin in three batches of Betula platyphylla bark extract. These results suggest that the developed HPLC method is simple, effective and could be utilized as a quality control method for Betula platyphylla bark products.

Development and Validation of a Robust LC-MS/MS Method for the Simultaneous Quantification of Doxifluridine and its Two Metabolites in Beagle Dog Plasma

  • Baek, In-Hwan;Chae, Jung-Woo;Chae, Han-Jung;Kwon, Kwang-Il
    • Bulletin of the Korean Chemical Society
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    • v.31 no.8
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    • pp.2235-2241
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    • 2010
  • A reverse-phase HPLC method with detection by mass spectrometry is described for the simultaneous determination of doxifluridine and its two active metabolites, 5-fluorouracil (5-FU) and 5-fluorouridine (5-FUrd), in beagle dog plasma. The optimal chromatographic separation was achieved on a Waters $Xterra^{(R)}$ $C_{18}$ column ($4.6{\times}250\;mm$ i.d., $5\;{\mu}m$ particle size) with a mobile phase of 0.1% formic acid in a mixture of 99% methanol and purified water (99:1, v/v). The developed method was validated in beagle dog plasma with a lowest limit of quantification of $0.05\;{\mu}g/mL$ for both doxifluridine and 5-FU, and $0.2\;{\mu}g/mL$ for 5-FUrd. Doxifluridine and its two metabolites were stable under the analysis conditions, and intra- and inter-day accuracies exceeded 92.87%, with a precision variability ${\leq}11.34%$ for each analyte. Additionally, the method for quantifying doxifluridine and its two metabolites, 5-FU and 5-FUrd, in beagle dog plasma was applied successfully to the analysis of pharmacokinetic samples.

A New Traffic Congestion Detection and Quantification Method Based on Comprehensive Fuzzy Assessment in VANET

  • Rui, Lanlan;Zhang, Yao;Huang, Haoqiu;Qiu, Xuesong
    • KSII Transactions on Internet and Information Systems (TIIS)
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    • v.12 no.1
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    • pp.41-60
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    • 2018
  • Recently, road traffic congestion is becoming a serious urban phenomenon, leading to massive adverse impacts on the ecology and economy. Therefore, solving this problem has drawn public attention throughout the world. One new promising solution is to take full advantage of vehicular ad hoc networks (VANETs). In this study, we propose a new traffic congestion detection and quantification method based on vehicle clustering and fuzzy assessment in VANET environment. To enhance real-time performance, this method collects traffic information by vehicle clustering. The average speed, road density, and average stop delay are selected as the characteristic parameters for traffic state identification. We use a comprehensive fuzzy assessment based on the three indicators to determine the road congestion condition. Simulation results show that the proposed method can precisely reflect the road condition and is more accurate and stable compared to existing algorithms.