• Title/Summary/Keyword: phase calibration

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Gastrointestinal and Hepatic First-pass Effects of Triflusal in Rats (흰쥐에서 트리플루살의 위장관 및 간 초회통과효과)

  • Cho, Hea-Young;Jeong, Tae-Jin;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.31 no.4
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    • pp.265-271
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    • 2001
  • In order to elucidate the influence of intestinal and hepatic first-pass effect on the pharmacokinetics of triflusal, the biotransformation of triflusal in the gastrointestinal tract and liver was designed. Moreover, we tried to establish an HPLC method applicable for bioassay and available to pharmacokinetics, not only with the simultaneous determination of triflusal and its active metabolite, 2-hydroxy-4-trifluoromethyl benzoic acid (HTB), but also with improving sensitivity. After the administration of triflusal (10 mg/kg) and HTB (10 mg/kg) into femoral vein, portal vein (only triflusal) and oral route (only triflusal), pharmacokinetic parameters were investigated from the plasma concentration-time profiles of triflusal and HTB in rats. An HPLC method was developed for the simultaneous determination of triflusal and HTB in rat plasma, urine and bile. The HPLC analysis was carried out using a C18 column and acetonitrile-methanol-water (25:10:65, v/v/v) as the mobile phase and UV detection at 234 nm. Furosemide was used as the internal standard. The calibration curves were linear over the concentration range $0.05-5.0\;{\mu}g/ml$ for triflusal and $0.2-200.0\;{\mu}g/ml$ for HTB with correlation coefficients greater than 0.999 and with intra-day or inter-day coefficients of variation not exceeding 10.0%. This assay procedure was applied to the study of metabolite pharmacokinetics of triflusal and HTB in rats. It was supposed that triflusal was almost metabolized in vivo because urinary and biliary excreted amounts of triflusal could be ignored as it was lower than 1.2% of the administered dose. According to the gastrointestinal and hepatic biotransformation pathways of triflusal, it was found that triflusal was hydrolyzed by about 5% in intestine and metabolized by about 53% in liver, and that the bioavailability of triflusal after oral administration of triflusal was 0.44, and also that the fraction of total elimination rate of triflusal which formed HTB in liver $(F_{mi},\;%)$ was about 98%. These results showed that triflusal was almost metabolized in liver, and the total elimination of triflusal in the body was dependent to the formation rate of HTB from triflusal in liver.

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Development of Analytical Methods of Hyperoside from Rosa canina L. (Rosa canina L. 중 hyperoside의 시험법 개발 연구)

  • Oh, Jae Myoung;Lee, Hwa Jung;Bahn, Kyeong Nyeo;Seo, Il Won;Lee, Young Joo;Lee, Jin Hee;Park, Ji Min;Kang, Tae Seok
    • Journal of Food Hygiene and Safety
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    • v.30 no.2
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    • pp.173-177
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    • 2015
  • Rosa canina L. is health functional food materials that can help to temporarily relieve symptoms of arthritis. This study has been conducted to develop and validate analytical methods for hyperoside of Rosa canina L.. Methods based on HPLC with ultraviolet detection (UVD) were established through instrumental analytical conditions, and the examination of data, such as domestic and foreign reliable methods and journals. HPLC UVD analysis using Capcell Pak $C_{18}$ MG II column at 353 nm was determined on test through the column, mobile phase. The validation has been performed on the method to determine linearity, accuracy, limits of quantification (LOQ) and repeatability for hyperoside. The method showed high linearity in the calibration curve at a coefficient of correlation ($R^2$) of 0.999, and the LOQ was $0.393{\mu}g/mL$. Relative standard deviation (RSD) values of data from repeatability precision was between 0.6 and 2.6%. Recovery rate test at hyperoside scored between 98 and 99%. These results indicate that the established HPLC method is very useful for the determination of hyperoside in Rosa canina L. to develop a health functional material.

Application of Laser-Induced Breakdown Spectroscopy (LIBS) for In-situ Detection of Heavy Metals in Soil (토양내 중금속 실시간 탐지를 위한 레이저 유도붕괴 분광법의 활용에 대한 소개)

  • Ko, Eun-Joung;Hamm, Se-Yeong;Kim, Kyoung-Woong
    • Economic and Environmental Geology
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    • v.40 no.5
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    • pp.563-574
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    • 2007
  • Laser induced breakdown spectroscopy (LIBS) is a recently developed analytical technique that is based upon the measurement of emission lines generated by atomic species close to the surface of the sample, thus allowing their chemical detection, identification and quantification. With powerful advantages of LIBS compared to the conventional analytical methodology, this technique can be applied in the detection of heavy metals in the field. LIBS allows the rapid analysis by avoiding laborious chemical steps. LES have already been applied for the determination of element concentration in a wide range of materials in the solid, liquid and gaseous phase with simplicity of the instrument and diversity of the analytical application. These feasibility of rapid multi elemental analysis are appealing proprieties for the in-situ analytical technique in geochemical investigation, exploration and environmental analysis. There remain still some limitations to be solved for LIBS to be applied in soil environment as an in-situ analytical technology. We would like to provide the basic principle related to the plasma formation and laser-induced breakdown of sample materials. In addition, the matrix effect, laser properties and the various factors affecting on the analytical signal of LIBS was dealt with to enhance understanding of LIBS through literature review. Ultimately, it was investigated the feasibility of LIBS application in soil environment monitoring by considering the basic idea to enhance the data quality of LIBS including the calibration method for the various effects on the analytical signal of LIBS.

Bioanalytical method validation for determination of arsenic speciation in dog plasma using HPLC-ICP/MS (Dog 혈장 중 HPLC-ICP/MS를 이용한 비소 화학종 분석법 검증)

  • Kim, Jong-Hwan;Kwon, Young Sang;Shin, Min-Chul;Kim, Su Jong;Seo, Jong-Su
    • Analytical Science and Technology
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    • v.29 no.5
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    • pp.234-241
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    • 2016
  • The approach presented in this article refers to the bioanalytical method validation for the detection and quantitative determination of arsenic species including arsenite (As(III)), arsenate (As(V)), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA) in dog plasma by high-performance liquid chromatography inductively coupled plasma mass spectrometry (HPLC-ICP/MS). The arsenic species were separated using an agilent As speciation column by a mobile phase of 2 mM sodium phosphate monobasic, 0.2 mM ethylenediaminetetraacetic acid disodium salt dehydrate, 10 mM sodium acetate, 3 mM sodium nitrate and 1 % ethyl alcohol at pH 11 (adjusted with 1M NaOH). The method validation experiment was obtained selectivity, linearity, accuracy, precision, matrix effect, recovery, system suitability, dilution integrity and various stabilities. All calibration curves showed good linearity (R2>0.999) within test ranges. The lower limit of quantitation (LLOQ) was 5 ng/mL for As(III), As(V) and DMA, and 20 ng/mL for MMA. The system suitability and dilution values were within 6.5 % and 7.7 %. Subsequently, the developed and validated HPLC-ICP/MS method was also successfully applied to determine the arsenic speciation in dog plasma samples, and the recoveries for the spiked samples were in the range of 91.5–102.2 %. Therefore, this method could be applied to the evaluation of arsenic exposure, health effect assessment and other bio-monitoring studies in biological samples.

Development and Validation of a Simultaneous Analytical Method for the Detection of Mefentrifluconazole and Triticonazole Fungicide in Agricultural Crops (농산물 중 메펜트리플루코나졸 및 트리티코나졸 살균제의 동시 분석법 개발 및 검증)

  • Park, Ji-Su;Lee, Han Sol;Lee, Su Jung;Shin, Hye-Sun;Shim, Jae-Han;Yun, Sang Soon;Jung, Yong-hyun;Oh, Jae-Ho
    • Korean Journal of Environmental Agriculture
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    • v.39 no.2
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    • pp.130-137
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    • 2020
  • BACKGROUND: Mefentrifluconazole and triticonazole are the triazole fungicides. The maximum residue levels for agricultural products need to be set up. Therefore, development of the official analytical method for determination of mefentrifluconazole and triticonazole residues from agricultural crops was necessary due to safety management, and then a simultaneous analytical method was developed for the determination of mefentrifluconazole and triticonazole in agricultural crops. METHODS AND RESULTS: Samples were extracted using acetonitrile and purified using dispersive solid phase extraction, and then detected with liquid chromatograph-tandem mass spectrometry (LC-MS/MS). Matrix-matched calibration curves (0.0025-0.25 ㎍/mL) were linear into a sample extract with r2>0.99. For validation, the recovery test was carried out at three fortification levels (LOQ, 10 LOQ and 50 LOQ) from agricultural samples. The results for mefentrifluconazole and triticonazole ranged between 92.3 to 115.3% and 91.4 to 108.5%, respectively and RSD (relative standard deviation) values were also below 6.0%. Furthermore, inter-laboratory was conducted to validate the method. CONCLUSION: All values were corresponded with the criteria ranges requested by both the CODEX (CAC/GL 40-1993, 2003) and MFDS guidelines (2016). Therefore, the proposed method can be used as an official analytical method for determination of mefentrifluconazole and triticonazole (triazole fungicides) in the Republic of Korea.

Determination of Bisphenols Migrating from Epoxy Can Coatings to Aqueous Food Simulants (통조림관 코팅제에서 식품유사용매로 이행되는 비스페놀류의 분석)

  • Kang, Kyung-Mo;Shin, Hyo-Sun
    • Korean Journal of Food Science and Technology
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    • v.32 no.3
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    • pp.570-577
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    • 2000
  • A method was presented for determination of bisphenol F(BPF), bisphenol A(BPA), bisphenol F diglycidyl ether(BFDGE) and bisphenol A diglycidyl ether(BADGE) in 3 aqueous-based food simulants (water, 4% acetic acid, 20% ethanol) by reverse-phase high performance liquid chromatography(RP-HPLC)with fluorescence detection and gas chromatography with mass selective detection(GC/MSD). All the calibration lines in the range of $5{\sim}800\;{\mu}g/L$ had correlation coefficients greater than 0.9998 and detection limits of less than $1.2\;{\mu}g$ bisphenols/L. Precision at $200\;{\mu}g/L$ was under 3.1%. Recoveries of bisphenols simultaneously spiked to aqueous food simulants exceeded 95% for BPF and BPA but about 80% for BFDGE and BADGE. However, recoveris of BFDGE and BPADGE respectively spiked increased upto 95%. Detection limits in recovery test were less than $0.40\;{\mu}g$ bisphenols/L. In migration test bisphenols were determined by RP-HPLC coupled with confirmation by GC/MSD. Can coatings of epoxy phenol, modified epoxy, epoxy ester phenol and thermoset vinyl were exposed to the 3 aqueous food simulants. BPF, BFDGE and BADGE were not detected in all the can coatings but BPA was detected in 4% acetic acid and 20% ethanol in all the can coatings except modified epoxy.

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A NEW HARDWARE CORRELATOR IN KOREA: PERFORMANCE EVALUATION USING KVN OBSERVATIONS

  • Lee, Sang-Sung;Oh, Chung Sik;Roh, Duk-Gyoo;Oh, Se-Jin;Kim, Jongsoo;Yeom, Jae-Hwan;Kim, Hyo Ryoung;Jung, Dong-Gyu;Byun, Do-Young;Jung, Taehyun;Kawaguchi, Noriyuki;Shibata, Katsunori M.;Wajima, Kiyoaki
    • Journal of The Korean Astronomical Society
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    • v.48 no.2
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    • pp.125-137
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    • 2015
  • We report results of the performance evaluation of a new hardware correlator in Korea, the Daejeon correlator, developed by the Korea Astronomy and Space Science Institute (KASI) and the National Astronomical Observatory of Japan (NAOJ). We conduct Very Long Baseline Interferometry (VLBI) observations at 22 GHz with the Korean VLBI Network (KVN) in Korea and the VLBI Exploration of Radio Astrometry (VERA) in Japan, and correlated the aquired data with the Daejeon correlator. For evaluating the performance of the new hardware correlator, we compare the correlation outputs from the Daejeon correlator for KVN observations with those from a software correlator, the Distributed FX (DiFX). We investigate the correlated flux densities and brightness distributions of extragalactic compact radio sources. The comparison of the two correlator outputs shows that they are consistent with each other within < 8%, which is comparable with the amplitude calibration uncertainties of KVN observations at 22 GHz. We also find that the 8% difference in flux density is caused mainly by (a) the difference in the way of fringe phase tracking between the DiFX software correlator and the Daejeon hardware correlator, and (b) an unusual pattern (a double-layer pattern) of the amplitude correlation output from the Daejeon correlator. The visibility amplitude loss by the double-layer pattern is as small as 3%. We conclude that the new hardware correlator produces reasonable correlation outputs for continuum observations, which are consistent with the outputs from the DiFX software correlator.

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.

Validation of Analytical Method of Marker Compounds in Extract of Pear Pomace as a Functional Health Ingredient (건강기능식품 원료로서 나주 배박 추출물의 지표성분 분석법 벨리데이션)

  • Cho, Eun-Jung;Bang, Mi-Ae;Cho, Seung-Sik
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.44 no.11
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    • pp.1682-1686
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    • 2015
  • This study was conducted to establish an HPLC analysis method for determination of marker compounds as part of materials standardization for development of health functional food materials from pear pomace. The quantitative determination method of caffeic acid and chlorogenic acid as marker compounds of pear pomace extract (PPE) was optimized by HPLC analysis using a C18 column ($5{\times}250mm$, $5{\mu}m$) with a 0.2% elution gradient of acetic acid and methanol as the mobile phase at a flow rate of 0.8 mL/min and detection wavelength of 330 nm. The HPLC/UV method was applied successfully to the quantification of marker compounds in PPE after validation of the method with linearity, accuracy, and precision. The method showed high linearity of the calibration curve with a coefficient of correlation ($R^2$) of 0.9999, and limit of detection and limit of quantification were $1.14{\mu}g/mL$ (caffeic acid) and $1.61{\mu}g/mL$ (chlorogenic acid) as well as $4.9{\mu}g/mL$ (caffeic acid) and $4.9{\mu}g/mL$ (chlorogenic acid), respectively. Relative standard deviation values from intra- and inter-day precision were less than 3.1% (caffeic acid) and 4.0% (chlorogenic acid), respectively. Recovery rates of caffeic acid and chlorogenic acid at 12.5, 25, and $50{\mu}g/mL$ were 93.66~106.32% and 97.33~105.68%, respectively. An optimized method for extraction of caffeic acid and chlorogenic acid in PPE was established through diverse extraction conditions, and the validation indicated that the method is very useful for evaluation of marker compounds in PPE to develop a health functional food material.

IGRINS First Light Instrumental Performance

  • Park, Chan;Yuk, In-Soo;Chun, Moo-Young;Pak, Soojong;Kim, Kang-Min;Pavel, Michael;Lee, Hanshin;Oh, Heeyoung;Jeong, Ueejeong;Sim, Chae Kyung;Lee, Hye-In;Le, Huynh Anh Nguyen;Strubhar, Joseph;Gully-Santiago, Michael;Oh, Jae Sok;Cha, Sang-Mok;Moon, Bongkon;Park, Kwijong;Brooks, Cynthia;Ko, Kyeongyeon;Han, Jeong-Yeol;Nah, Jakyuong;Hill, Peter C.;Lee, Sungho;Barnes, Stuart;Park, Byeong-Gon;T., Daniel
    • The Bulletin of The Korean Astronomical Society
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    • v.39 no.1
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    • pp.52.2-52.2
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    • 2014
  • The Immersion Grating Infrared Spectrometer (IGRINS) is an unprecedentedly minimized infrared cross-dispersed echelle spectrograph with a high-resolution and high-sensitivity optical performance. A silicon immersion grating features the instrument for the first time in this field. IGRINS will cover the entire portion of the wavelength range between 1.45 and $2.45{\mu}m$ accessible from the ground in a single exposure with spectral resolution of 40,000. Individual volume phase holographic (VPH) gratings serve as cross-dispersing elements for separate spectrograph arms covering the H and K bands. On the 2.7m Harlan J. Smith telescope at the McDonald Observatory, the slit size is $1^{\prime\prime}{\times}15^{\prime\prime}$. IGRINS has a $0.27^{\prime\prime}$ pixel-1 plate scale on a $2048{\times}2048$ pixel Teledyne Scientific & Imaging HAWAII-2RG detector with SIDECAR ASIC cryogenic controller. The instrument includes four subsystems; a calibration unit, an input relay optics module, a slit-viewing camera, and nearly identical H and K spectrograph modules. The use of a silicon immersion grating and a compact white pupil design allows the spectrograph collimated beam size to be 25mm, which permits the entire cryogenic system to be contained in a moderately sized rectangular vacuum chamber. The fabrication and assembly of the optical and mechanical hardware components were completed in 2013. In this presentation, we describe the major design characteristics of the instrument and the early performance estimated from the first light commissioning at the McDonald Observatory.

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