• Title/Summary/Keyword: N-R Method

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Multi-Residue Analysis of 18 Dye Residues in Animal Products by Liquid Chromatography-Tandem Mass Spectrometry

  • Park, Hyunjin;Kim, Joohye;Kang, Hui-Seung;Cho, Byung-Hoon;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.35 no.2
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    • pp.109-117
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    • 2020
  • This study aimed to develop an analytical method for determination of 18 dyes in livestock and fishery products by liquid chromatograph-tandem mass spectrometry (LC-MS/MS). The developed method was validated for linearity, accuracy, limit of quantifications (LOQ) and recovery based on the CODEX guideline (CAC/GL-71). Target matrices (beef, pork, chicken, egg, milk, flatfish, eel, and shrimp) were extracted using acetonitrile (containing 1% of acetic acid) and then, purified with C18 and primary secondary amine (PSA). Calibration linearity was obtained (r2>0.98) and LOQs were 0.002 mg/kg in animal products. The recoveries of dyes were ranged from 63 to 112% and relative standard deviations (RSDs, %) were less than 15%. The residues of 18 dyes were investigated in real samples (n=124) collected from retail markets in South Korea. As a result, a total of seven samples showed positive results for target analytes in fish samples. However, there was no violation according to the maximum residue limits set by the Korean Food Code. The proposed method will be used for routine analysis of dye residues in livestock and fishery products.

Aberration Retrieval Algorithm of Optical Pickups Using the Extended Nijboer-Zernike Approach (확장된 네이보어-제르니케 방법에 의한 광픽업의 파면수차 복원 알고리즘)

  • Jun, Jae-Chul;Chung, Ki-Soo;Lee, Gun-Kee
    • Journal of the Institute of Convergence Signal Processing
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    • v.11 no.1
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    • pp.32-40
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    • 2010
  • In this work, the method of acquiring the pupil function of optical system is proposed. The wavefront aberration and the intensity distribution of pupil can be analysed with the pupil function. This system can be adopted to the manufacturing line of optical pickup directly and also has good performance to analysing various property of optical instrument. It is one kind of inverse problem to get pupil functions by 3D beam data. The extended Nijboer-Zernike(ENZ) approach recently proposed by Netherlands research group is adopted to accompany to solve these inverse problem. The ENZ approach is one of a aberration retrieval method for which numerous approaches are available. But this approach is new in the sense that it use the highly efficient representation of pupil functions by means of their Zernike coefficients. These coefficients are estimated by using matching procedure in the focal region the theoretical 3D intensity distribution and measured 3D intensity distribution. The algorithm that can be applied more general circumstance such as high-numerical aperture instrument is developed by modifying original ENZ approach. By these scheme, MS windows based GUI program is developed and the good performance is verified with generated 3D beam data.

Determination of alkylphenol ethoxylate in water by high performance liquid chromatography/electrospray ionization/mass spectrometry (HPLC/ESI/MS를 이용한 물 중의 알킬페놀에톡실레이트 분석)

  • Lee, Jeongae;Park, Song-Ja;Chung, Bong Chul
    • Analytical Science and Technology
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    • v.17 no.3
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    • pp.263-270
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    • 2004
  • A method is described for the analysis of short-chain alkylphenol ethoxylates (APEOs), 4-octylphenol-di-ethoxylate (OP2EO) and 4-nonylphenol-di-ethoxylate (NP2EO), in drinking water or wastewater using reversed phase high-performance liquid chromatography with electrospray ionization mass spectrometry. The solvent system was water and methanol containing $10{\mu}M$ trifluoroacetic acid as an ionization solvent. We acidified 1 L of water samples to less than pH 2 with concentrated $H_2SO_4$ and loaded onto Sep-Pak $C_{18}$, and eluted with acetone. The calibration of OP2EO and NP2EO was performed for the concentration range from 20 to 500 ng/L and the correlation coefficients were 0.999 and 0.990, respectively. The limits of detection were 20 ng/L (OP2EO) and 50 ng/L (NP2EO) at a signal-to-noise ratio of 3. Accuracy and precision of this analytical method were 85.8 ~ 122.1% and 8.2 ~ 18.8%, respectively. The proposed method allowed a sensitive and rapid detection of OP2EO and NP2EO and it could be applied for monitoring of APEOs from environmental samples.

Determination of Niacin in Infant Formula by Solid-phase Clean-up and HPLC with Photodiode Array Detector (고체상 정제 및 HPLC/PDA에 의한 영유아식 중 나이아신의 분석)

  • Hong, Jee-Eun;Kim, Mi-Ran;Cheon, Sang-Hee;Chai, Jung-Young;Park, Eun-Ryong;Mun, Chun-Sun;Gwak, In-Shin;Kim, Ok-Hee;Lee, Kwang-Ho
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.38 no.3
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    • pp.359-363
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    • 2009
  • This study was performed to establish a rapid and simple analytical method for niacin (nicotinic acid and nicotinamide) using HPLC. A pretreatment method for the extraction and clean-up of niacin in infant formula sample and an instrumental condition for HPLC were optimized. Niacin was extracted by 5 mM hexanesulfonate with ultrasonication for 30 min. For the clean-up of the sample, the extract was applied to a HLB cartridge, and then niacin was eluted from the cartridge using 5 mL of 80% methanol after washing with 5 mL of n-hexane. The total recoveries were $83{\sim}104%$ and relative standard deviation were in the range of $1.5{\sim}3.5%$ during the extraction and clean-up process. Niacin was determined by gradient elution with sodium hexanesulfonate/methanol buffer as a mobile phase and a photodiode array detector (260 nm). It showed a high linearity between the content of niacin and the peak area ($r^2$=1.000) in the range of $0.02{\sim}10.0$ mg/L of nicotinic acid and nicotinamide. The detection limit was 0.02 mg/L (0.2 mg/kg in the sample). The method was successfully applied for the determination of niacin in infant formula. Total niacin contents were in the range of $53.5{\sim}140.3$ mg/kg.

Development of the Simultaneous Analysis of 36 Sulfonylurea Herbicide Residues in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 제초제 Sulfonylurea계 36종 동시 시험법 개발)

  • Su Jung Lee;Jung Mi Lee;Gui Hyun Jang;Hyun-Kyung Kim;Ji Young Kim
    • Korean Journal of Environmental Agriculture
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    • v.42 no.2
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    • pp.139-151
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    • 2023
  • Sulfonylurea herbicides are widely used in agriculture because they have a long residual period and high selectivity. An analytical method was developed using QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) technique for simultaneous determination of sulfonylurea herbicide residues in agricultural products by liquid chromatography tandem mass spectrometry and for establishment MRL (Maximum Residue Limit) of those herbicides in Korea. Extraction was performed using acetonitrile containing 0.1% formic acid with MgSO4 (anhydrous magnesium sulfate) and NaCl (sodium chloride) and the extract was cleaned up using MgSO4 and C18 (octadecyl). The matrix-matched calibration curves were composed of 7 concentration levels from 0.001 to 0.25 mg/kg and their coefficients of determination (R2) exceeded 0.99. The recoveries of three spiking levels (LOQ, 10LOQ, 50LOQ, n=5) were in the range of 71.7-114.9% with relative standard deviations of less than 20.0% for all the five agriculture products. All validation values met criteria of the European Union SANTE/11312/2021 guidelines and Food and Drug Safety Evaluation guidelines. Therefore, the proposed analytical method was accurate, effective, and sensitive for sulfonylurea herbicide residues determination in agricultural commodities.

Development and Validation of the Analytical Method for Oxytetracycline in Agricultural Products using QuEChERS and LC-MS/MS (QuEChERS법 및 LC-MS/MS를 이용한 농산물 중 Oxytetracycline의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Cho, Myong-Shik;Jung, ong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.3
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    • pp.227-234
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    • 2019
  • An analytical method was developed for the determination of oxytetracycline in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). After the samples were extracted with methanol, the extracts were adjusted to pH 4 by formic acid and sodium chloride was added to remove water. Dispersive solid phase extraction (d-SPE) cleanup was carried out using $MgSO_4$ (anhydrous magnesium sulfate), PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed with LC-MS/MS using ESI (electrospray ionization) in positive ion MRM (multiple reaction monitoring) mode. The matrix-matched calibration curves were constructed using six levels ($0.001{\sim}0.25{\mu}g/mL$) and coefficient of determination ($r^2$) was above 0.99. Recovery results at three concentrations (LOQ, $10{\times}LOQ$, and $50{\times}LOQ$, n=5) were from 80.0 to 108.2% with relative standard deviations (RSDs) less than of 11.4%. For inter-laboratory validation, the average recovery was in the range of 83.5~103.2% and the coefficient of variation (CV) was below 14.1%. All results satisfied the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for oxytetracycline determination in agricultural commodities. This study could be useful for safety management of oxytetracycline residues in agricultural products.

Studies on the Xylans of Tropical Hardwoods (III) - Property of Purified Xylan - (열대산활엽수재(熱帯産闊葉樹材)의 Xylan에 관(関)한 연구(硏究) (III) - 정제(精製) Xylan의 성상(性状) -)

  • Lee, Jong Yoon
    • Journal of Korean Society of Forest Science
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    • v.56 no.1
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    • pp.77-81
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    • 1982
  • The property of four tropical hardwoods were analyzed. xylans, extracted with 24% of potassium hydroxide and purified according to ethanol titration procedure, were examined for Pn, the uronic acid, methoxyl groups and acetyl groups content. Only mangrove, whose xylan content is similar to that of hardwoods in the temperature zone, had the ratio of units of xylose residue to the units of uronic acid residue as high as that of hardwoods in the temperature zone. Content of methoxyl groups showed the same result as uronic acid residue content. Various hemicellulose including D-xylose residue were contained in xylans extracted by D M S O. Acetyl groups content was compressed of 5.4% of M D X and 6.8% of R D X. Xylans unextracted by D M S O had acetyl groups. Pn measured by the viscosity method was about 200 and similar to the hardwood xylans of temperature zone. DPn calculated by uronic acid residue was similar to that of tropical zone.

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Changes in Vegetation Characteristics Over Time in the Isolated Forests of the Urban Areas: A Case Study on the Mt. Hwangyeong, Busan Metropolitan City (도시 내 고립된 임지의 경시적 식생특성 변화: 부산광역시 황령산을 사례로)

  • Cho, Jae Hyong;Park, Chan Ryul;Oh, Jeong Hak;Kim, Jun Soo;Cho, Hyun Je
    • Journal of Korean Society of Forest Science
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    • v.105 no.3
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    • pp.284-293
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    • 2016
  • In order to assess th changes in vegetation characteristics over time in the forest-lands which is isolated by urbanization, vegetation surveys based on the Braun-Blanquet phytosociological method was carried out in 1996 and 2015 on Mt. Hwangyeong located in the center of Busan metropolitan city, South Korea. The number of vegetation types based on floristic composition showed no significant changes, the vegetation units under the community levels was more or less represents the difference. the average total vegetation cover and average number of species per unit area ($100m^2$) was increased 16% and 2 species, respectively. The relative importance value (RIV) for each tree species, Quercus spp. like as Q. mongolica and Q. serrata was decreased, while the warmth-tolerant trees, evergreen broad-leaved trees, and mesophyte like Lindera erythrocarpa, Styrax japonica, Osmanthus heterophyllus, and Stephanandra incisa was increased significantly. Changes of the life form spectrums of vascular plants did not substantially, hemicryptophyte(H) and therophyte (Th) was decreased, while nanophanerophyte(N) was increased significantly. Also through the creating of large-scale vegetation map (based on physiognomic vegetation types) was compared the spatial distribution characteristics of each vegetation types.

The Types of Extended-Spectrum ${\beta}$-Lactamases Isolated from Suyeong Sewage Disposal Plant, Busan Environmental Corporation (부산 수영공공하수처리시설에서 분리된 광범위 항균제 베타락 탐 분해효소(Extended-Spectrum ${\beta}$-Lactamase, ESBL) 유형)

  • Kim, Gun-Do;Lee, Hun-Ku
    • Korean Journal of Microbiology
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    • v.46 no.1
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    • pp.38-45
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    • 2010
  • The study performed to identify the type of ESBL against strains which are producing extendedspectrum ${\beta}$-lactamases and isolated from sewage in Suyeong sewage disposal plant, Busan Environmental Corporation. By the standard activated sludge method, Suyeong sewage disposal plant purify living and lavatory sewage gathering from the northeast Busan and the facility purify total 550,000 tons of living sewage disposal a day. 14 strains were isolated by double disk synergy test and the third generation cepha-antibiotics test. Indole, methyl-red, Voges-Proskauer, Simmon's citrate, decarboxylasedihydrolase and sugar-fermentation tests identified as Klebsiella pneumoniae (n=4) and Escherichia coli (n=10). Plasmid-mediated transmission test against isolated 14 strains proved 11 strains transmitted resistance to recipient E. coli J53 (sodium $azide^R$, $ceftazidime^S$). 9 strains of conjugant were expressed ESBL genes transferred from parental strain but 2 conjugants did not expressed. The type of ESBL from each strain was determined by isoelectric focusing points, DNA and amino acids sequencing. The results indicated that the types of ESBL transmitted to recipient E. coli J53 were TEM-1, the parental TEM type and SHV-12 type.

Hydrophobic Cyclodextrin Derivatives as a Sustained Release Carrier of Azidothymidine (아지도싸이미딘의 지속성방출형담체로서의 소수성시클로덱스트린유도체)

  • Seo, Bo-Youn;Park, Gee-Bae;Lee, Kwang-Pyo
    • Journal of Pharmaceutical Investigation
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    • v.26 no.2
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    • pp.71-82
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    • 1996
  • This study has been undertaken to evaluate hydrophobic cyclodextrin(CD) derivatives as a sustained release carrier of azidothymidine(AZT), AZT, which has potent activity against AIDS and AIDS-related complex as thymidine analogue, has been reported that it has significant toxicity and short half life. Therefore, it is necessary to design sustained release oral dosage form to avoid undesirable side effects attributable to an excessive plasma concentration and to reduce the frequency of administration of AZT. Inclusion complexes of AZT with $acetyl-{\beta}-cyclodextrin\;(AC{\beta}CD)$ and $triacetyl-{\beta}-cyclodextrin(TA{\beta}CD)$ were prepared by solvent evaporation method. Interactions of AZT with CD were investigated by Differential Scanning Calorimetry(DSC) and Infrared Spectrophotometry(IR). The decreasing order of water solubilities of AZT and AZT-CD inclusion complexes were as follows; $AZT\;(27.873{\pm}0.015,mg/ml)\;>\;AZT-AC{\beta}CD\;(3.377{\pm}0.003)\;>\;AZT-TA{\beta}CD\;(2.528{\pm}0.001)$. Partition coefficients of $AZT-AC{\beta}CD\;and;\AZT-TA{\beta}CD$ inclusion complexes were increased by 1.27-fold, 1.54-fold in pH 1.2 and 1.32-fold, 1.47-fold in pH 6.8 in comparison with that of AZT. The mean dissolution time (MDT, min) which represents the rapidity of dissolution rate of AZT, $AZT-AC{\beta}CD,\;AZT-TA{\beta}CD$ were 5.12, 14.02 and 19.38 min in pH 1.2 and 2.52, 15.19 and 18.19 min in pH 6.8. AZT was very rapidly and completely dissolved in pH 1.2 and pH 6.8 within 5 minutes. But AZT-CD inclusion complexes showed the sustained release pattern in comparison with AZT alone. The simultaneous in situ nasal and jejunal recirculation study to compare the intrinsic absorptivity and the property of absorption sites revealed that the absorption of $AZT-TA{\beta}CD\;(N:35.35{\pm}1.08%,\;J:27.47{\pm}1.18%)$ was more than that of $AZT\;(N:16.89{\pm}2.25%,\;J:15.86{\pm}2.33%)$. The above results suggest that $TA{\beta}CD$ which is a hydrophobic cyclodextrin may serve as sustained release carrier with absorption enhancing effect.

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