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Establishment for analytical method of methanol in wet wipes by headspace gas chromatography (가스크로마토그래프-헤드스페이스를 이용한 물휴지 중 메탄올 정량법 확립 연구)

  • Choi, Yongkyu;Baek, Eunji;Min, Chungsik;Lee, Rheeda;Park, Soonyoung;Ahn, Jaehyung;Kim, Sangseop;Hong, Seonghwa;Kim, Younglim
    • Analytical Science and Technology
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    • v.29 no.5
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    • pp.242-247
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    • 2016
  • This research aims to set up and validate methods of analyzing the methanol in wet wipes and verifies the analysis methods that applied to the wet wipes. We used Headspace (HS) Gas Chromatography (GC) - Flame Ionization Detector (FID) to the establish analysis method of methanol in wet wipes and optimized heating temperature, heating time, GC conditions with column. The result indicated that 3 mL of sample in 20 mL headspace vial can be equilibrated efficiently in headspace sampler at 70 ℃ for 10 min and sample was measured by GC with spli injection mode(10:1). The results show that linearity from 1 to 100 ppm was over R2 0.9995, precision was RSD 1.83 % and accuracy(recovery rate) was 105.44 (±1.05 %) on water matrix and wet wipes matrix removed non-woven fabric. Also, monitoring results of total 20 cosmetics on the market, from 0.00017 to 0.00156 % of methanol was detected from wet wipes.

Development of high performance liquid chromatography assay method of diosmin capsules (디오스민 캡슐의 HPLC 분석법의 개발)

  • Shim, Dae Hyun;Shin, Dong Han;Truong, Quoc Ky;Mai, Xuan Lan;Kang, Jong-Seong;Woo, Mi Hee;Na, Dong-Hee;Chun, In-Koo;Kim, Kyeong Ho
    • Analytical Science and Technology
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    • v.29 no.6
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    • pp.277-282
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    • 2016
  • British Pharmacopoeia (BP 2013), the United States Pharmacopoeia (USP 39) and the Korean Pharmacopoeia (KP XI) contain monographs for the quality control of raw diosmin using high performance liquid chromatography (HPLC). However, official monographs detailing pharmaceutical formulations for diosmin are not available in foreign pharmacopoeias. In the KP XI, ultraviolet-visible (UV-Vis) spectroscopy-which is less specific than HPLC-is reported for the testing of diosmin capsules. In this study, we present an alternative HPLC assay for such testing that is more specific than UV-Vis methods. 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 ($r^2$>0.999), while the RSDs for intra- and inter-day precision were 0.15-0.29 % and 1.05-1.74%, respectively. Accuracies ranged from 101.2-103.2 %, while the retention time and peak area RSDs were 0.37 % and 0.06 %, respectively. Additionally, the plate number and asymmetry factor values for diosmin were 3591.293 and 1.35, respectively. Since the intermediate-precision and robustness of the assay were satisfactory, this method will be a valuable addition to the Korean Pharmacopoeia (KP XI).

Analytical method validation and monitoring of levulinic acid in soy sauce and their application to food (간장 및 이를 활용한 식품의 레불린산 분석방법 검증 및 모니터링)

  • Kim, Dan-Bi;Kim, Sunyoung;Lee, Sanghee;Yoo, Miyoung
    • Analytical Science and Technology
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    • v.30 no.5
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    • pp.295-302
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    • 2017
  • This study presents a method validation for extraction and quantitative analysis of levulinic acid in soy sacues using high performance liquid chromatograph-photodiode array detector (HPLC-PDA). The levulinic acid in samples were extracted with distilled water, and then purified with C18 Sep-Pak cartridge. The calibration curves showed good linearity (R > 0.999) in a relatively wide concentration range ($2.5-400{\mu}g/mL$). Mean recoveries and relative standard deviation (RSD) of levulinic acid spiked in soy sauce samples at different spiking levels ($2.5-400{\mu}g/mL$; 6 point). Recoveries were 87.58-97.26 % with RSD less than 15 %, and limit of detection (LOD) and limit of quantification (LOQ) were 0.64 and $1.64{\mu}g/mL$, respectively. According to monitoring result with the established method, levulinic acid was found in 43 of 59 domestic commercial soy sauces, soy sauce based sauces and seasoned meats. The contamination levels were 0.44-1.23 mg/mL for soy sauces, 0.03-0.83 mg/mL for soy sauce based sauces and 8.43-38.94 mg/mL for seasoned meats. The results indicated to be rapidly and accurately qualifying levulinic acid and can be used as a suitable quality control method for soy sauce and soy sauce related commodities.

Analytical Methods on the Determination of Active Ingredients for Hair Nourisher Products (HPLC를 이용한 양모제 유효성분의 동시분석법)

  • Kwon, Kyoung-Jin;Kim, Do-Jung;Kim, Sang-Seop;Choi, Yu-Bin;Kim, Mi-Jeong;Choi, Myeong-Sin;Cho, Bo-Kyung;Kim, Dong-Sup
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.36 no.3
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    • pp.167-174
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    • 2010
  • The hair nourisher products are used for prevention of hair loss and classified as quasi-drug in Korea. As concerns about hair loss has been increased, the demand for hair nourisher products has been growing. It is difficult to analyze their main ingredients because they contain various ingredients including natural plant extracts, vitamins, preservatives and exfoliators. The purpose of this study was to develop and validate simultaneous analytical methods of active ingredients in hair nourisher products such as nicotinamide, tocopherol, salicylic acid, dexpanthenol and benzyl nicotinate by HPLC. The active ingredients were separated on a $C_{18}$ column by using acetonitrile/phosphate buffer as a mobile phase, and detected at UV 220, 270 and 300 nm. The calibration curve showed linearity in the range of $12.5{\sim}800\;{\mu}g/mL$ and the recoveries were 97.3 ~ 103.5 % (RSD 0.9 ~ 2.8 %) in liquid matrix and 101.9 ~ 115.9 % (RSD 0.7 ~ 7.7 %) in shampoo matrix. Validated method was applied to hair nourisher products obtained from distribution market. Fortunately, all samples met their criteria. This study might be expected to provide the method for determining active ingredients in hair nourisher products and lead to promote a rapid market entry.

A Study of the Clinical Application of Thermography in Musculoskeletal Disease (근골격계(筋骨格系) 영역(領域)에서 Thermography의 임상적(臨床的) 활용(活用)에 대(對)한 고찰(考察))

  • Shin, Hyun-Taeg;Chung, Seok-Hee;Lee, Jong-Soo;Kim, Sung-Soo;Shin, Hyun-Dae
    • The Journal of Dong Guk Oriental Medicine
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    • v.8 no.2
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    • pp.47-67
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    • 2000
  • The purpose of this study is to assess the usefulness of thermography in patients with musculoskeletal disease. Thermography is noninvasive, easy to reading, objective and physiologic instrument by measuring and imaging infrared energy emitted from skin surface. Thermography can show the skin temperature changes in various conditions of the body with musculoskeletal disease. This literature review was done for the usefulness of thermography in diagnosing musculoskeletal disease. In conclusion, thermography was adapted in radiculopathy, MPS, peripheral neuropathy, RSD, Raynaud's phenomen, TMJ dysfunction, etc. It was useful as a secondary diagnostic method in those diseases, also possible as a primary diagnostic method in RSD, Raynaud's phenomen. And, it might be reliable tool for estimating disease procedure and consequence after treatment. But, the objectivity of the reading and the development of the operating method are required for further adaptation in musculoskeletal disease.

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Multiresidue Analysis of 240 Pesticides in Apple and Lettuce by QuEChERS Sample Preparation and HPLC-MS/MS Analysis (QuEChERS 전처리법과 HPLC-MS/MS 기기분석을 이용한 사과와 상추 중 240종 농약의 동시분석)

  • Kwon, Hye-Young;Kim, Chan-Sub;Park, Byung-Jun;Jin, Yong-Duk;Son, Kyung-Ae;Hong, Su-Myeong;Lee, Je-Bong;Im, Geon-Jae
    • The Korean Journal of Pesticide Science
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    • v.15 no.4
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    • pp.417-433
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    • 2011
  • The study tested QuEChERS (quick, easy, cheap, effective, rugged and safe) sample preparation and HPLC-MS/ MS analysis for measurement of pesticide residues in fruit and vegetable. 240 kinds of pesticides spiked at three levels of 90, 45, 9 ng/g in lettuce and apple. For QuEChERS sample preparation, graphitized carbon black (GCB) was used for only lettuce in dispersive-SPE as absorbent. Matrix-matched standard calibration was used for quantitative analysis of HPLC-MS/MS. 218 pesticides (91%) in apple and 207 pesticides (86%) in lettuce showed recoveries in the range of 70~120% with $RSD{\leq}20%$. The lowest calibrated level (LCL) were 4.5 ng/g for 192 pesticides, 9 ng/g for 42 pesticides, 45 ng/g for 3 pesticides and 3 pesticides were not detected at all concentration levels. The results showed that the QuEChERS sample preparation and HPLC-MS/MS analysis can be applied to multi-residue analysis of pesticides in vegetables and fruits.

Competitive Extraction of Chlorinated Solvents by Headspace SPME GC/FID (Headspace SPME GC/FID를 이용한 Chlorinated Solvents의 경쟁적 추출효과에 관한 연구)

  • An, Sangwoo;Kim, Youngju;Chun, Sukyoung;Lee, Sijin;Park, Jaewoo;Chang, Soonwoong
    • Journal of the Korean GEO-environmental Society
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    • v.11 no.5
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    • pp.61-67
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    • 2010
  • In this study, Solid-phase microextraction (SPME) with GC/FID was studied as a possible alternative to liquid-liquid extraction for the analysis of chlorinated solvents (PCE and TCE) and these by-products (cis-DCE, VC, and Ethylene). Experimental parameters affecting the SPME process (such as kind of fibers, adsorption time, desorption time, volume ratio of sample to headspace, salt addition, and magnetic stirring) were optimized. Experimental parameters such as CAR/PDMS, adsorption time of 20 min, desorption time of 5 min at $250^{\circ}C$, headspace volume of 50mL, sodium chloride (NaCl) concentration of 25% combined with magnetic stirring were selected in optimal experimental conditions for analysis of chlorinated solvents and these by-products. The general affinity of analytes to CAR/PDMS fiber was high in the order PCE>TCE>cis-DCE>VC>Ethylene. The linearity of $R^2$ for chlorinated solvents and these by-products was from 0.912 to 0.999 when analyte concentrations range from $10{\mu}g/L$ to $500{\mu}g/L$, respectively. The relative standard deviation (% RSD) were from 2.1% to 3.6% for concentration of $500{\mu}g/L$ (n=5), respectively. Finally, the limited of detection (LOD) observed in our study for chlorinated solvents and these by-products were from $0.5{\mu}g/L$ to $10{\mu}g/L$, respectively.

Capillary Electrophoretic Method for the Determination of (+)-Catechin, (-)-Epicatechin in Grape Seed Ethanol Extract (포도종실 에탄올 추출물에 함유된 (+)-카테킨, (-)-에피카테킨의 모세관 전기영동법에 의한 분석)

  • Choi, One-Kyun;Chung, Yang-Seop;Chung, Ha-Yull
    • Korean Journal of Food Science and Technology
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    • v.37 no.4
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    • pp.513-518
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    • 2005
  • Capillary electrophoresis (CE) method was developed to determine (+)-catechin and (-)-epicatechin contents in grape seed ethanol extract. CE separation was achieved using 100 mM phosphate and borate buffer at pH 6.0 as background electrolyte and fused silica capillary with 50 microns x 375 microns O.D. (effective length 20.0cm) maintained at $25^{\circ}C$. The applied voltage was 10kV, and detection was performed by DAD at 210 nm, Two catechins were well separated within 6 min with repeatability of <0.8% RSD for migration time and <2.0% RSD for peak area, and correlation coefficients higher than 0.994 were obtained from 58.0 to 174.0 mg/L with detection limit of 0.035 mg/L. Separated compounds were successfully determined. CE method was easy to handle and showed good reproducibility. CE method was compared with conventional coloring and HPLC methods, and main advantages of CE method were low amount of sample required, simple pre-sample treatment, good recovery rate, and short analysis time.

Analysis of Synthetic Fragrances (SFs) in Water Using Stir Bar Sorptive Extraction (SBSE) and GC-MS/MS (교반막대 추출법과 GC-MS/MS를 이용한 수중의 합성 향물질류 분석)

  • Seo, Chang-Dong;Son, Hee-Jong;Yoom, Hoon-Sik;Choi, Jin-Taek;Ryu, Dong-Choon;Kwon, Ki-Won;Jang, Seung-Ho
    • Journal of Korean Society of Environmental Engineers
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    • v.36 no.6
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    • pp.387-395
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    • 2014
  • A highly sensitive analytical method based on stir bar sorptive extraction (SBSE) technique and gas chromatography/tandem mass spectrometry (GC-MS/MS) has been developed, allowing the simultaneous multi-analyte determination of 11 synthetic fragrances (SFs) in water samples. The stir bar coated with polydimethylsiloxane (PDMS) was added to 40 mL of water sample at pH 3 and stirred at 1,100 rpm for 120 min. Other SBSE parameters (salt effect and presence of organic solvent) were optimised. The method shows good linearity (coefficients > 0.990) and reproducibility (RSD < 10.9%). The extraction efficiencies were above 83% for all the compounds. The limits of detections (LOD) and limits of quantification (LOQ) were 2.1~4.1 ng/L and 6.6~12.9 ng/L, respectively. The developed method offers the ability to detect 11 SFs at ultra-low concentration levels with only 40 mL of sample volume. Matrix effects in tap water, river water, wastewater treatment plant (WWTP) final effluent water and seawater were investigated and it was shown that the method is suitable for the analysis of trace level of 11 SFs. The method developed in the present study has the advantage of being rapid, simple, high-sensitive and both user and environmentally friendly.

The Study on the Production Method of Stepwise Dilution Gas for Odor Analysis with Orifice Tubes (오리피스 튜브에 의한 단계별 냄새 분석용 희석가스의 제조방법에 관한 연구)

  • Kim, Han-Soo;Lee, Seok-Jun;Kim, Sun-Tae
    • Journal of Korean Society of Environmental Engineers
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    • v.35 no.2
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    • pp.137-143
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    • 2013
  • This study is to develop the production method of stepwise dilution gas for the evaluation of complex odor concentration by orifice tube. The basic orifice tube for 10 and 30 times of dilution sample was made at first, and with the combination of the basic orifice tubes we can continuously manufacture the stepwise dilution sample gas for air dilution sensory test ; 10, 30, 100, 300, 1,000, 3,000 times etc. The hole size of orifice tube was 0.84 mm for 10 times of dilution sample, and was 0.34 mm for 30 times. Dilution sample gas made with the basic orifice tube have an excellent reproducibility, 2%RSD. In addition, over 90% of correlation was shown between the sample made by the orifice tube and the sample by the syringe dilution method. Because there was no concentration drift of dilution gas with changes of connected pump flow, the basic orifice tube could be mounted directly with a vacuum suction box, and could be used simply as a tool for the evaluation of odor, especially on site.