• Title/Summary/Keyword: Method detection limits

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Development of an analytical method for the quantification of oleanonic acid from mastic gum using HPLC/PDA

  • Hak-Dong Lee;Chang-Dae Lee;So Yeon Choi;Sanghyun Lee
    • Journal of Applied Biological Chemistry
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    • v.66
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    • pp.67-72
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    • 2023
  • A simple and accurate method was developed for the quantitative analysis of oleanonic acid (OA) from mastic gum. The analysis was carried out using reverse-phase high-performance liquid chromatography combined with a photodiode array detector (HPLC/PDA). Our optimized method was validated by measuring various parameters, using an INNO C18 column fitted with a gradient elution system. The results revealed limits of detection and quantification of 0.34 and 1.042 ㎍/mL, respectively. The OA calibration curve exhibited excellent linearity over the concentration range of 0.0625 to 2.0 mg/mL, with r2 =0.9996. Accuracy tests revealed a high recovery rate of 99.44-103.66%, with precision values below 0.15%. These results suggest that the present analytical method can identify and quantify OA in mastic gum with high precision. The HPLC approach developed in this study might be applied to routine analyses and large-scale extraction procedures for OA content quantification.

Simple and Rapid Detection of Vancomycin-Resistance Gene from Enterococci by Loop-Mediated Isothermal Amplification

  • Baek, Yun Hee;Hong, Seung Bok;Shin, Kyeong Seob
    • Biomedical Science Letters
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    • v.26 no.3
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    • pp.149-156
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    • 2020
  • We developed a simple and rapid method for detecting vancomycin resistance genes, such as vanA and vanB, using loop-mediated isothermal amplification (LAMP). To identify not only vancomycin resistance genes, but also the genus Enterococcus, primers were designed for vanA, vanB, and 16S rRNA. Screening for vancomycin susceptibility in Enterococcus was performed using Etest (bioMérieux Inc). The results of the LAMP assay were compared to those of real-time RT-PCR. The optimal conditions for the LAMP assay were 65℃ for 60 min. The detection limits of the LAMP assay for vanA, and vanB were 2 × 102 copies/reaction. Compared to RT-PCR, the sensitivities and specificities of LAMP for 16S rRNA, vanA, and vanB were 100/100%, 100/100%, and 100/100%, respectively. The vanA genotype-vanB phenotype accounted for 57.5% (46/80) of the vancomycin-resistant Enterococci samples collected from 2016 to 2019. In conclusion, the LAMP assay developed in this study showed high sensitivity and specificity for vancomycin-resistant genes. Moreover, due to the simplicity and rapidity of the LAMP assay, its use can be very useful in clinical microbiology laboratories.

Recognizing Human Facial Expressions and Gesture from Image Sequence (연속 영상에서의 얼굴표정 및 제스처 인식)

  • 한영환;홍승홍
    • Journal of Biomedical Engineering Research
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    • v.20 no.4
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    • pp.419-425
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    • 1999
  • In this paper, we present an algorithm of real time facial expression and gesture recognition for image sequence on the gray level. A mixture algorithm of a template matching and knowledge based geometrical consideration of a face were adapted to locate the face area in input image. And optical flow method applied on the area to recognize facial expressions. Also, we suggest hand area detection algorithm form a background image by analyzing entropy in an image. With modified hand area detection algorithm, it was possible to recognize hand gestures from it. As a results, the experiments showed that the suggested algorithm was good at recognizing one's facial expression and hand gesture by detecting a dominant motion area on images without getting any limits from the background image.

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Identification of Higenamine nad its Metabolites in Rat by Gas Chromatography/Mass Spectrometry

  • Ryu, Jae-chun;Song, Yun-Seon;Kim, Myung-Soo;Cho, Jung-Hyuck;Yunchoi, Hye-Sook
    • Archives of Pharmacal Research
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    • v.16 no.3
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    • pp.213-218
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    • 1993
  • ($\pm$)-Higenamine is known as a cardiotonic principle of aconite root (root of Aconitum spp., Ranunculaceae). A simple and sensitive detection method for higenamine was developed by using gas chromatography-mass spectrometry (GC/MS). The recovery of higenamine after extraction and concentration with XAD-2 resin column was around 95% from rat biological fluids such as bile, plasma and urine. The limits of detection of higenamine in these biological fluids were approximately 0.1 ng/ml each. It has well been suggested that tetrahydroisoquinolines possessing catechol moiety such as higenamine should be subjected to the catechol-O-methyl transferase (COMT) activity in vivo. We detected two major peaks of presumed metabolites of higenamine in the total ion chromatogram obtained from the rat urine sample after the oral adminstration of ($\pm$)-higenamine. The scan mass spectrum of one of the metabolties coincided with those obtained from coclaurine $(C_6$-O-methyl higenamine) and those of the other metabolite are suggestive of isococlaurine $(C_7$-O-methyl higenamine).

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Detection of Abnormal Ship Operation using a Big Data Platform based on Hadoop and Spark (하둡 및 스파크 기반 빅데이터 플랫폼을 이용한 선박 운항 효율 이상 상태 분석)

  • Lee, Taehyeon;Yu, Eun-seop;Park, Kaemyoung;Yu, Seongsang;Park, Jinpyo;Mun, Duhwan
    • Journal of the Korean Society of Manufacturing Process Engineers
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    • v.18 no.6
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    • pp.82-90
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    • 2019
  • To reduce emissions of marine pollutants, regulations are being tightened around the world. In the shipbuilding and shipping industries, various countermeasures are being put forward. As there are limits to applying countermeasures to ships already in operation, however, it is necessary for these vessels to use energy efficiently. The sensors installed on ships typically gather a very large amount of data, and thus a big data platform is needed to manage and analyze the data. In this paper, we build a big data analysis platform based on Hadoop and Spark, and we present a method to detect abnormal ship operation using the platform. We also utilize real ship operation data to discuss the data analysis experiment.

A Study on the Analysis of Polycyclic Aromatic Hydrocarbons by RPLC/DAD (I) (RPLC/DAD를 이용한 Polycyclic Aromatic Hydrocarbon류의 분석에 관한 연구(I))

  • Lee, Won;Hong, Jee-Eun;Park, Song-Ja;Pyo, Hee Soo
    • Analytical Science and Technology
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    • v.10 no.5
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    • pp.315-324
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    • 1997
  • The retention behaviors of 16 PAHs and 4 nitro-PAHs were studied with several parameters involved numbers of carbon atoms, F factor, aqueous solubility, L/B ratio, and numbers of interfering hydrogen atom pairs on the chemical structures of PAHs by using reversed-phase liquid chromatography/diode array detection method (RPLC/DAD) and gradient elution method. It was obtain that the log k' for most of PAHs with increasing the number of carbon and the F factor in their molecules. Chromatographic retention of PAH isomers and nitro-PAHs were examined with aqueous solubility, L/B ratio and number of interfering hydrogen atom pairs. As a result of comparison with these factors and retention times, it was found that those solutes having larger aqueous solubilities and greater L/B ratios were retained longer on stationary phase. This tendency was also occured in the molecules having the more number of interfering hydrogen atom pairs. Detection limits of PAHs which were obtained with three times measurements by RPLC/DAD were in the range of 100~500ng/mL and method detection limit(MDL) for water sample were in the range of 0.1~0.5ng/mL.

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Extraction of Phthalate Esters in Environmental Water Samples Using Layered-Carbon Magnetic Hybrid Material as Adsorbent Followed by Their Determination with HPLC

  • Wang, Weina;Wu, Qiuhua;Zang, Xiaohuan;Wang, Chun;Wang, Zhi
    • Bulletin of the Korean Chemical Society
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    • v.33 no.10
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    • pp.3311-3316
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    • 2012
  • In this paper, a layered-carbon-$Fe_3O_4$ (LC-$Fe_3O_4$) hybrid material was synthesized through a facile one-pot solvothermal method and used as the adsorbent for the preconcentration of some phthalate esters (dimethyl phthalate, diethyl phthalate, diallyl phthalate, diisobutyl phthalate and benzyl butyl phthalate) in water samples. The effects of the adsorbent dosage, extraction time, the solution pH and salinity on the adsorption of the phthalate esters (PAEs) were investigated. The magnetic nanocomposite adsorbent could remove and enrich the PAEs from water samples efficiently. After the adsorption, the analytes were desorbed and then determined by high performance liquid chromatography-ultraviolet detection. Under the optimum conditions, the enrichment factors of the method for the analytes were in the range from 161 to 180. A linear response with peak area as the quantification signal was observed in the concentration range from 0.5 to $100ng\;mL^{-1}$. The limits of detection (S/N = 3) of the method were between 0.08 and $0.1ng\;mL^{-1}$. The method was suitable for the determination of trace phthalate esters in environmental water samples.

Determination of 8-iso-PGF as Oxidative Stress Marker in Human Urine by High Performance Liquid Chromatography with Tandem Mass Spectrometry (LC/MS/MS를 이용한 산화성 스트레스 지표로써 소변 중 8-iso-PGF 분석)

  • Kho, Young-Lim;Lee, Eun-Hee;Chae, Hong-Jae;Choi, Kyung-Ho;Paik, Do-Myung
    • Journal of Environmental Health Sciences
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    • v.36 no.1
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    • pp.44-51
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    • 2010
  • This study aimed to develop analytical method for 8-isoprostanes as biomarkers for oxidative stress with LC/MS/MS technique and to apply the method for human urine samples. Analyzed compounds for urinary oxidative stress markers were 7 stereo-isomers of prostaglandins and the internal standard (iso-$PGF_{2{\alpha}}-d_4$) was used to adjust the recovery rate. The method for determining urinary iso-$PGF_{2{\alpha}}$ consisted of solid phase extraction and LC/MS/MS detection. Separation of isomers of prostaglandins completed by porous graphitic carbon column and buffer solution. Detection limits for urinary markers of oxidative stress, iso-$PGF_{2{\alpha}}$ with LC/MS/MS were 0.01 ng/ml by S/N ratio 3 and 0.028 ng/ml by calculated as to FDA method. The recovery (92.8~101.9%) and precision (8.8~20.7%) of analysis were feasible for detecting iso-$PGF_{2{\alpha}}$ in real human urine samples. We detected 4 isomers of prostaglandins in human urine samples. Mean (standard deviation) of urinary iso-$PGF_{2{\alpha}}$ concentration were 0.231 (0.117) ng/mg creatinine for smoking group and 0.154 (0.082) ng/mg creatinine for non-smoking group.

A Study of Analytical Method for Ethylene and Low Weight Hydrocarbons (LWHC) using Thermal Desorption and Gas Chromatography-Flame Ionization Detector with (TD-GC-FID) (저온열탈착기술을 이용한 에틸렌 및 저분자 탄화수소 분석방법 연구)

  • Kim, Bo-Won;Kim, Ki-Hyun;Kim, Yong-Hyun;Ahn, Jeong-Hyeon
    • Journal of Korean Society for Atmospheric Environment
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    • v.30 no.1
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    • pp.77-87
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    • 2014
  • In this study, an experimental approach to measure a suite of low weight hydrocarbons was investigated with an emphasis on ethylene (EL) along with many others (ethane (EA), propane (PA), propylene (PL), n-butane (BA), acetylene (AL), methyl acetylene (ML)). Their concentrations were quantified using GC-FID system equipped with thermal desorption (TD) system. The TD-based analysis was conducted using both Link Tube/Thermal Desorber (LT/TD) method and Modified Injection through a Thermal Desorption (MITD) method. The results of these analyses were evaluated in a number of respects. The system allowed the detection of all compounds except methane with the mean response factor (RF) of 10.28 (EA) to 11.94 (PL). The method detection limits of target compounds were seen in the range of 0.027 (ML) to 0.146 ng (BA). The emission flux of some environmental samples (fruits), when measured using a small flux chamber system, fell in the range of 0.14 (AL: Kiwi) to $181ng{\cdot}g^{-1}{\cdot}hr^{-1}$ (EL: Apple Peel). The results of this study confirm that the experimental approach developed in this study allows to accurately measure emissions of low weight hydrocarbons (LWHC) like ethylene from various natural and man-made source processes.

Simultaneous Determination of Baicalin and Glycyrrhizin in Eul-Ja-Tang by HPLC/DAD

  • Lee, Mi-Kyeong;Lee, Ki-Yong;Kim, Seung-Hyun;Park, Jung-Hyun;Cho, Jung-Hee;Oh, Mi-Hyun;Baek, Ju-Hyun;Kim, Hyo-JIn;Kim, Young-Choong;Sung, Sang-Hyun
    • Natural Product Sciences
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    • v.14 no.3
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    • pp.147-151
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    • 2008
  • A high performance liquid chromatographic (HPLC) method for the simultaneous determination of marker constituents, baicalin and glycyrrhizin was established for the quality control of traditional herbal medicinal preparation, Eul-Ja-Tang (EJT). Separation and quantification were successfully achieved with a Waters XTerra RP18 column ($5{\mu}m$, 4.6 mm I.D. ${\times}$ 150 mm) by gradient elution of a mixture of acetonitrile and water containing 0.03% phosphoric acid (pH 2.03) at a flow rate of 1.0 mL/min. The diode-array UV/VIS detector (DAD) was used for the detection and the wavelength for quantification was set at 250 nm. The presence of baicalin and glycyrrhizin in this decoction was ascertained by retention time, spiking with each authentic standard and UV spectrum. Both baicalin and glycyrrhizin showed good linearity ($r^2$ > 0.999) in a relatively wide concentration ranges. The R.S.D. for intra-day and inter-day precision was less than 5% and the limits of detection (LOD) were about 30 ng. The mean recovery of each compound was 99.5 - 101.2% with R.S.D. values less than 4.0%. This method was successfully applied to the determination of contents of baicalin and glycyrrhizin in three commercial products of EJT, which resulted in the difference in the contents of these compounds. These results suggest that the developed HPLC method is simple, effective and could be readily utilized as a quality control method for commercial EJT products.