• Title/Summary/Keyword: ultra-precision

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Simultaneous Determination of 8 Preservatives (6 Parabens, 2-Phenoxyethanol, and Chlorphenesin) in Cosmetics by $UPLC^{TM}$ ($UPLC^{TM}$를 이용한 화장품 중 보존제 8종(파라벤 6종, 페녹시에탄올, 클로페네신)의 동시분석)

  • Park, Jeong-Eun;Lee, So-Mi;Jeong, Hye-Jin;Chang, Ih-Seop
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.33 no.4
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    • pp.263-267
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    • 2007
  • Parabens are used in nearly all types of cosmetics and toiletries because they are formulated well and have broad spectrum of activity, interness, low costs and excellent chemical stability in relation to pH. 2-phenoxyethanol and chlorphenesin are common preservatives which are usually used in combination with parabens in cosmetics. Toxicity of parabens is generally low but application of parabens to damaged or broken skin has resulted in sensitization. Moreover, the possibility of their estrogenic potential, anesthetic effects and reproductive toxicity has been reported. Consequently there are some regulations in use of parabens. And the maximum permitted concentrations of chlorphenesin and 2-phenoxyethanol in cosmetic products are authorized by the same reasons. So it is important to control and estimate the amount of parabens in products. In this article, we proposed a valid method for the simultaneous determination of 8 preservatives including parabens in a short time using ultra performance liquid $chromatography^{TM}\;(UPLC^{TM})$. Separation of eight components was achieved in less than 10 min and resolutions were reasonable (USP resolution ${\geqq}\;2$). And limit of detection and quantification were evaluated. The method was suitably validated for specificity, linearity, precision (repeatability, intermediate precision) and accuracy for assay (recovery) based on International conference on harmonisation (ICH) guideline. The method was applicable to analysis of preservatives in cosmetic products.

Method Development for Determination of Chlorogenic Acid and Arbutin Contents in Fruits by UHPLC-MS/MS (UHPLC-MS/MS를 이용한 과일류 중 클로로젠산 및 알부틴 동시분석법 개발)

  • Choi, Young-Ju;Jeon, Jong-Sup;Kim, Woon-Ho;Jung, You-Jung;Ryu, Ji-Eun;Choi, Jong-Chul;Chae, Kyung-Suk;Lee, Jin-Hee;Do, Young-Sook;Park, Young-Bae;Yoon, Mi-Hye
    • Journal of Food Hygiene and Safety
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    • v.34 no.5
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    • pp.413-420
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    • 2019
  • In this study, a sample preparation method and a simultaneous determination method by ultra-high performance liquid chromatography coupled with tandem mass spectrometry for 9 isomers of chlorogenic acid and arbutin in fruits were developed. The samples were extracted using 90% methanol (pH 3.0), with the solutions being shaken and then sonicated for 10 min each. After centrifugation at 4,000 rpm for 10 min, the extraction was concentrated under a vacuum at $40^{\circ}C$ using a vacuum evaporator. The residue was dissolved in 5 mL of 5% methanol and filtered through a $0.45{\mu}m$ membrane before UHPLC-MS/MS analysis. The separations were performed on a C18 column with gradient elution of water (containing 0.1% formic acid) and methanol (containing 0.1% formic acid). The specificity, linearity, limit of detection, limit of quantification, accuracy, and precision of the proposed methods were also evaluated.

A Study on the Development of Ultra-precision Small Angle Spindle for Curved Processing of Special Shape Pocket in the Fourth Industrial Revolution of Machine Tools (공작기계의 4차 산업혁명에서 특수한 형상 포켓 곡면가공을 위한 초정밀 소형 앵글 스핀들 개발에 관한 연구)

  • Lee Ji Woong
    • Journal of Practical Engineering Education
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    • v.15 no.1
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    • pp.119-126
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    • 2023
  • Today, in order to improve fuel efficiency and dynamic behavior of automobiles, an era of light weight and simplification of automobile parts is being formed. In order to simplify and design and manufacture the shape of the product, various components are integrated. For example, in order to commercialize three products into one product, product processing is occurring to a very narrow area. In the case of existing parts, precision die casting or casting production is used for processing convenience, and the multi-piece method requires a lot of processes and reduces the precision and strength of the parts. It is very advantageous to manufacture integrally to simplify the processing air and secure the strength of the parts, but if a deep and narrow pocket part needs to be processed, it cannot be processed with the equipment's own spindle. To solve a problem, research on cutting processing is being actively conducted, and multi-axis composite processing technology not only solves this problem. It has many advantages, such as being able to cut into composite shapes that have been difficult to flexibly cut through various processes with one machine tool so far. However, the reality is that expensive equipment increases manufacturing costs and lacks engineers who can operate the machine. In the five-axis cutting processing machine, when producing products with deep and narrow sections, the cycle time increases in product production due to the indirectness of tools, and many problems occur in processing. Therefore, dedicated machine tools and multi-axis composite machines should be used. Alternatively, an angle spindle may be used as a special tool capable of multi-axis composite machining of five or more axes in a three-axis machining center. Various and continuous studies are needed in areas such as processing vibration absorption, low heat generation and operational stability, excellent dimensional stability, and strength securing by using the angle spindle.

Method Validation and Quantification of Lutein and Zeaxanthin from Green Leafy Vegetables using the UPLC System (UPLC를 이용한 lutein과 zeaxanthin의 분석법 검증 및 엽채류에서의 정량적 평가)

  • Kim, Suna;Kim, Ji-Sun
    • Korean Journal of Food Science and Technology
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    • v.44 no.6
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    • pp.686-691
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    • 2012
  • The objective of this research is to present method development and validation for the simultaneous determination of lutein and zeaxanthin using ultra performance liquid chromatography (UPLC). Also, rapid quantification was performed on six green leafy vegetables (Allium tuberosum, Aster scaber, Hemerocallis fulva, Pimpinella brachycarpa, Sedum sarmentosum and Spinacia oleracea) that are commonly consumed in Korea. Separation and quantification were successfully achieved with a Waters Acquity BEH C18 ($50{\times}2.1mm$, $1.7{\mu}m$) column by 85% methanol within 5 min. Two compounds showed good linearity ($r^2$ > 0.9968) in $1-150{\mu}g/mL$. Limit of detection (LOD) and quantification (LOQ) for lutein and zeaxanthin were 1.7 and 5.1 g/mL and 2.1 and 6.3 g/mL, respectively. The RSD for intra- and inter-day precision of each compound was less than 10.69%. The recovery of each compound was in the range of 91.75-105.13%. Aster scaber and Spinacia oleracea contained significantly higher amounts of lutein ($4.06{\pm}0.24$ and $3.97{\pm}0.10mg$/100 g of fresh weight), respectively.

Determination of Arsenic in Water by ICP-DRC/MS (ICP-DRC/MS를 이용한 수중의 비소 측정)

  • Jeong, Gwan-Jo;Kim, Dok-Chan;Park, Hyeon
    • Journal of Korean Society of Environmental Engineers
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    • v.28 no.6
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    • pp.620-625
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    • 2006
  • In this investigation, an ICP-DRC/MS method to measure arsenic with ultra-trace concentration without any interference by the compounds such as $^{40}Ar^{35}Cl^+\;and\;^{40}Ca^{35}Cl^+$, which disturb the precise measurement of arsonic was described. Thus, the oxgen was introduced into the dynamic reaction cell as reaction gas and reacted with arsenic ion created in plasma gas, $AsO^+$ was formed and detected with m/z of 91 by ICP-MS. It resulted in better detection limit than the old method with m/z of 75($As^+$). The optimum condition for oxygen supply as the reaction gas was 0.5 mL/min. The analytical features of the method are as follows: detection limit of $0.02{\mu}g/L$, precision(RSD) of 3.4%, and recovery of 96%. Arsenic in the water samples from the tributary streams to the Han River and the main stream of Paldang were analyzed with this method to identify the characteristics in its distribution. The concentration of As ranged from 0.53 to $1.26{\mu}g/L$. We could measure As with very low concentration, less than $1.0{\mu}g/L$, with excellent reproducibility. The method developed is expected to be applied to analyze As of the samples from sea water, food, and domestic and industrial waste water which have high concentration of Cl and/or Ca.

Development of a flower support for real flower decoration Automatic Production System (생화 장식 꽃받침 자동 생산 시스템 개발)

  • Song, Myung-Seok;Kim, Man-Joong;Kim, Seon-Bong;Ji, Peng;Ryuh, Beom-Sahng
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.19 no.7
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    • pp.63-71
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    • 2018
  • A flower support was developed for real flower decoration automation production system using an ultrasonic wave sealer to automatically produce a system. Because a flower support for real flower decoration that was produced manually could not meet the needs of the consumers, this study developed an automated manufacturing system to increase productivity. A flower support for real flower decoration was constructed using a cap consisting of plastic and plate made from non-woven fabric. The guide was designed to transport the cap to the ultrasonic wave sealer and optimal guide was developed from the test according to the material and shape. To produce the entire system, the guides and accessories were weighed and appropriate motors and pulleys were calculated. Control of the automation production system was based on a PCB board, which increased the reliability and security, and a remote controller with manual and automatic modes was prepared. After development, tests of the transfer precision and repetition accuracy revealed an X-axis of 2.7mm, a Y-axis of 1 mm, and a repetition of 0 mm. The productivity was also checked. The automated machine worked 8 hours/day to make 35 supports and 70 Therefore, the automatic system produces 200% more output than manual work

Classification and Comparative Analysis of the Contents of Acorus species and Anemone altaica by UPLC-PDA Analysis (UPLC-PDA를 이용한 창포류의 분류 및 함량 분석)

  • Jo, Ji Eun;Lee, A Yeong;Kim, Hyo Seon;Moon, Byeong Cheol;Ji, Yunui;Chun, Jin Mi;Kim, Ho Kyoung
    • Korean Journal of Food Science and Technology
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    • v.45 no.3
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    • pp.279-284
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    • 2013
  • A quantitative method using ultra performance liquid chromatography with a photodiode array detector (UPLCPDA) was established for the analysis of 2 major plant metabolites: ${\beta}$-asarone and ${\alpha}$-asarone from Acorus gramineus, A. tatarinowii, A. calamus and Anemone altaica, and their contents are compared with other herbs of Acorus species. The method was validated according to the International Conference on harmonization (ICH) guideline for validation of analytical procedures with respect to precision, accuracy, and linearity. The average content of ${\beta}$-asarone in Acorus gramineus was significantly higher than that in others, with the second highest concentration observed in A. tatarinowii, and only a trace amounts found in A. calamus and Anemone altaica. In contrast, the average content of ${\alpha}$-asarone in A. calamus was the highest, followed by that in Acorus gramineus and A. tatarinowii. principle component analysis (PCA) confirmed that ${\beta}$-asarone and ${\alpha}$-asarone content differed among the species. These results suggest that this UPLC-PDA method can be considered as good quality control criteria for Acorus gramineus.

Full validation of high-throughput bioanalytical method for the new drug in plasma by LC-MS/MS and its applicability to toxicokinetic analysis

  • Han, Sang-Beom
    • Proceedings of the Korean Society of Toxicology Conference
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    • 2006.11a
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    • pp.65-74
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    • 2006
  • Modem drug discovery requires rapid pharmacokinetic evaluation of chemically diverse compounds for early candidate selection. This demands the development of analytical methods that offer high-throughput of samples. Naturally, liquid chromatography / tandem mass spectrometry (LC-MS/MS) is choice of the analytical method because of its superior sensitivity and selectivity. As a result of the short analysis time(typically 3-5min) by LC-MS/MS, sample preparation has become the rate- determining step in the whole analytical cycle. Consequently tremendous efforts are being made to speed up and automate this step. In a typical automated 96-well SPE(solid-phase extraction) procedure, plasma samples are transferred to the 96-well SPE plate, internal standard and aqueous buffer solutions are added and then vacuum is applied using the robotic liquid handling system. It takes only 20-90 min to process 96 samples by automated SPE and the analyst is physically occupied for only approximately 10 min. Recently, the ultra-high flow rate liquid chromatography (turbulent-flow chromatography)has sparked a huge interest for rapid and direct quantitation of drugs in plasma. There is no sample preparation except for sample aliquotting, internal standard addition and centrifugation. This type of analysis is achieved by using a small diameter column with a large particle size(30-5O ${\mu}$m) and a high flow rate, typically between 3-5 ml/min. Silica-based monolithic HPLC columns contain a novel chromatographic support in which the traditional particulate packing has been replaced with a single, continuous network (monolith) of pcrous silica. The main advantage of such a network is decreased backpressure due to macropores (2 ${\mu}$m) throughout the network. This allows high flow rates, and hence fast analyses that are unattainable with traditional particulate columns. The reduction of particle diameter in HPLC results in increased column efficiency. use of small particles (<2 urn), however, requires p.essu.es beyond the traditional 6,000 psi of conventional pumping devices. Instrumental development in recent years has resulted in pumping devices capable of handling the requirements of columns packed with small particles. The staggered parallel HPLC system consists of four fully independent binary HPLC pumps, a modified auto sampler, and a series of switching and selector valves all controlled by a single computer program. The system improves sample throughput without sacrificing chromatographic separation or data quality. Sample throughput can be increased nearly four-fold without requiring significant changes in current analytical procedures. The process of Bioanalytical Method Validation is required by the FDA to assess and verify the performance of a chronlatographic method prior to its application in sample analysis. The validation should address the selectivity, linearity, accuracy, precision and stability of the method. This presentation will provide all overview of the work required to accomplish a full validation and show how a chromatographic method is suitable for toxirokinetic sample analysis. A liquid chromatography/tandem mass spectrometry (LC-MS/MS) method developed to quantitate drug levels in dog plasma will be used as an example of tile process.

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Fabrication and characterization of $WSi_2$ nanocrystals memory device with $SiO_2$ / $HfO_2$ / $Al_2O_3$ tunnel layer

  • Lee, Hyo-Jun;Lee, Dong-Uk;Kim, Eun-Kyu;Son, Jung-Woo;Cho, Won-Ju
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.02a
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    • pp.134-134
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    • 2011
  • High-k dielectric materials such as $HfO_2$, $ZrO_2$ and $Al_2O_3$ increase gate capacitance and reduce gate leakage current in MOSFET structures. This behavior suggests that high-k materials will be promise candidates to substitute as a tunnel barrier. Furthermore, stack structure of low-k and high-k tunnel barrier named variable oxide thickness (VARIOT) is more efficient.[1] In this study, we fabricated the $WSi_2$ nanocrystals nonvolatile memory device with $SiO_2/HfO_2/Al_2O_3$ tunnel layer. The $WSi_2$ nano-floating gate capacitors were fabricated on p-type Si (100) wafers. After wafer cleaning, the phosphorus in-situ doped poly-Si layer with a thickness of 100 nm was deposited on isolated active region to confine source and drain. Then, on the gate region defined by using reactive ion etching, the barrier engineered multi-stack tunnel layers of $SiO_2/HfO_2/Al_2O_3$ (2 nm/1 nm/3 nm) were deposited the gate region on Si substrate by using atomic layer deposition. To fabricate $WSi_2$ nanocrystals, the ultrathin $WSi_2$ film with a thickness of 3-4 nm was deposited on the multi-stack tunnel layer by using direct current magnetron sputtering system [2]. Subsequently, the first post annealing process was carried out at $900^{\circ}C$ for 1 min by using rapid thermal annealing system in nitrogen gas ambient. The 15-nm-thick $SiO_2$ control layer was deposited by using ultra-high vacuum magnetron sputtering. For $SiO_2$ layer density, the second post annealing process was carried out at $900^{\circ}C$ for 30 seconds by using rapid thermal annealing system in nitrogen gas ambient. The aluminum gate electrodes of 200-nm thickness were formed by thermal evaporation. The electrical properties of devices were measured by using a HP 4156A precision semiconductor parameter analyzer with HP 41501A pulse generator, an Agillent 81104A 80MHz pulse/pattern generator and an Agillent E5250A low leakage switch mainframe. We will discuss the electrical properties for application next generation non-volatile memory device.

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The Possibility of Environmental Paraquat Exposure (파라콰트의 환경성 노출 가능성)

  • Oh, Se-Hyun;Choi, Hong-Soon;You, Ho-Young;Park, Jun-Ho;Song, Jae-Seok
    • Journal of agricultural medicine and community health
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    • v.36 no.4
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    • pp.218-226
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    • 2011
  • Objectives: Paraquat (PQ) is a widely used ionic pesticide that is fatal when ingested accidentally or for suicidal purposes. It is thought that chronic exposure of PQ is related with the development of Parkinson's disease, but epidemiological studies have not yet confirmed that theory. This study attempted to estimate the possibility of environmental PQ exposure through soil and water. Materials and Methods: We analyzed the amount of decomposed PQ solution in wet soil after exposure to ultraviolet light. An artificial rainfall condition was simulated over soil sprayed with PQ to measure the amount of eluted PQ. In addition, PQ was diluted in water from three differently rated rivers and the changes in PQ concentration were measured after ultraviolet exposure over one month. High performance liquid chromatography/ultra violet detection was used to analyze the concentrations of PQ. Results: In the method we used, the recovery rate of PQ showed a precision rate less than 5%, an accuracy greater than 88%, and the calibration equation was y=5538.8x-440.01($R^2$=0.9985). There were no significant differences in the concentrations of PQ obtained from the three specimens over a 1-week period. From the PQ-sprayed soil, the artificial rainfall conditions showed no PQ elution over a 1-month period, and there was no significant differences in PQ concentrations according to ultraviolet exposure among the three samples. Conclusions: PQ remains well adsorbed naturally in soil. However, it may still exist in an integrated state for a long time in the hydrosphere, so the possibility of PQ exposure through drinking water cannot be disqualified.