• Title/Summary/Keyword: 2-D analytical method

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Analytical Method for Determination of Laccaic Acids in Foods with HPLC-PDA and Monitoring (식품 중 락카인산 성분 분리정제를 통한 분석법 확립 및 실태조사)

  • Jae Wook Shin;Hyun Ju Lee;Eunjoo Lim;Jung Bok Kim
    • Journal of Food Hygiene and Safety
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    • v.38 no.5
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    • pp.390-401
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    • 2023
  • Major components of lac coloring include laccaic acids A, B, C, and E. The Korean Food Additive Code regulates the use of lac coloring and prohibits its use in ten types of food products including natural food products. Since no commercial standards are available for laccaic acids A, B, C, and E, a standard for lac pigment itself was used to separate laccaic acids from the lac pigment molecule. A standard for each laccaic acid was then obtained by fractionation. To obtain pure lac pigment for use in food by High performance Liquid Chromatography Photo Diode Array (PDA), a C8 column yielded the best resolution among various tested columns and mobile phases. A qualitative analytical method using High Performance Liquid Chromatography (HPLC) Tandem Mass(LC-MS/MS) was developed. The conditions for fast and precise sample preparation begin with extraction using methanol and 0.3% ammonium phosphate, followed by concentration. The degree of precision observed for the analyses of ham, tomato juice and Red pepper paste was 0.3-13.1% (Relative Standard Deviation (RSD%)), degree of accuracy was 90.3-122.2% with r2=0.999 or above, and recovery rate was 91.6-114.9%. The limit of detection was 0.01-0.15 ㎍/mL, and the limits of quantitation ranged from 0.02 to 0.47 ㎍/mL. Lac pigment was not detected in 117 food products in the 10 food categories for which the use of lac pigment is banned. Multiple laccaic acids were detected in 105 food products in 6 food categories that are allowed to use lac color. Lac pigment concentrations range from 0.08 to 16.67 ㎍/mL.

Studies on the analysis of phytin by the Chelatometric method (Chelate 법(法)에 의(依)한 Phytin 분석(分析)에 관(關)한 연구(硏究))

  • Shin, Jai-Doo
    • Applied Biological Chemistry
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    • v.10
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    • pp.1-13
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    • 1968
  • Phytin is a salt(mainly calcium and magnesium) of phytic acid and its purity and molecular formula can be determined by assaying the contents of phosporus, calcium and magnesium in phytin. In order to devise a new method for the quantitative analysis of the three elements in phytin, the chelatometric method was developed as follows: 1) As the pretreatment for phytin analysis, it was ashfied st $550{\sim}600^{\circ}C$ in the presence of concentrated nitric acid. This dry process is more accurate than the wet process. 2) Phosphorus, calcium and megnesium were analyzed by the conventional and the new method described here, for the phytin sample decomposed by the dry process. The ashfied phytin solution in hydrochloric acid was partitioned into cation and anion fractions by means of a ration exchange resin. A portion of the ration fraction was adjusted to pH 7.0, followed by readjustment to pH 10 and titrated with standard EDTA solution using the BT [Eriochrome black T] indicator to obtain the combined value of calcium and magnesium. Another portion of the ration fraction was made to pH 7.0, and a small volume of standard EDTA solution was added to it. pH was adjusted to $12{\sim}13$ with 8 N KOH and it was titrate by a standard EDTA solution in the presence of N-N[2-Hydroxy-1-(2-hydroxy-4-sulfo-1-naphytate)-3-naphthoic acid] diluted powder indicator in order to obtain the calcium content. Magnesium content was calculated from the difference between the two values. From the anion fraction the magnesium ammonium phosphate precipitate was obtained. The precipitate was dissolved in hydrochloric acid, and a standard EDTA solution was added to it. The solution was adjusted to pH 7.0 and then readjusted to pH 10.0 by a buffer solution and titrated with a standard magnesium sulfate solution in the presence of BT indicator to obtain the phosphorus content. The analytical data for phosphorus, calcium and magnesium were 98.9%, 97.1% and 99.1% respectively, in reference to the theoretical values for the formula $C_6H_6O_{24}P_6Mg_4CaNa_2{\cdot}5H_2O$. Statical analysis indicated a good coincidence of the theoretical and experimental values. On the other hand, the observed values for the three elements by the conventional method were 92.4%, 86.8% and 93.8%, respectively, revealing a remarkable difference from the theoretical. 3) When sodium phytate was admixed with starch and subjected to the analysis of phosphorus, calcium and magnesium by the chelatometric method, their recovery was almost 100% 4) In order to confirm the accuracy of this method, phytic acid was reacted with calcium chloride and magnesium chloride in the molar ratio of phytic: calcium chloride: magnesium chloride=1 : 5 : 20 to obtain sodium phytate containing one calcium atom and four magnesium atoms per molecule of sodium phytate. The analytical data for phosporus, calcium and magnesium were coincident with those as determine d by the aforementioned method. The new method employing the dry process, ion exchange resin and chelatometric assay of phosphorus, calcium and magnesium is considered accurate and rapid for the determination of phytin.

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On the Evaluation of Physical Distribution Service in Ports (항만물류서비스의 평가에 관하여)

    • Journal of Korean Port Research
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    • v.10 no.2
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    • pp.17-29
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    • 1996
  • It is required to consider pricing and non-pricing factors and external economy in order to achieve the objects of physical distribution system in a port. Recently, among the three factors, much attention has been paid to non-pricing factor in the system. Although physical distribution service in a port(PDSP)has been frequently mentioned in documents and literature related to port and shipping studies, few study on it has not been systematically and scientifically made due to the following problems; $\circ$ there are not proper criteria to evaluate level and quality of PDSP and as a result it is difficult to set up a unified standard for doing so. $\circ$ algorithms to evaluate problems with complex and ambiguous attributes and multiple levels in PDSP are not available. This thesis aims to establish a paradigm to evaluate PDSP and to abvance existing decision making methods to deal with complex and ambiguous problems in PDSP. To tackle the first purpose, extensive and thorough literature survey was carried out on general physical distribution service, which is a corner stone to handle PDSp. In addition, through interviews and questionnaire to the expert, it have extracted 82 factors of physical distribution service in a port. They have been classified into 6 groups by KJ method and each group defined by the expert's advice as follows; a. Potentiality b. Exactness c. safety d. Speediness e. Convenience f. Linkage Prior to the service evaluation, many kinds of its attributes must be identified on the basis of rational decision owing to complexity and ambiguity inherent in PDSP. An analytical hierarchy process (AHP) is a method to evaluate them but it is not applicable to PDSP that have property of non-additivity and overlapped attributes. Therefore, probablility measure can not be used to evaluate PDSP but fuzzy measure is required. Hierarchical fuzzy integral method, which is merged AHP with fuzzy measure, is also not effective method to evaluate attributes because it has vary complicated way to calculate fuzzy measure identification coefficient of attributes. A new evaluation algorithm has been introduced to solve problems with multi-attribute and multi-level hierarchy, which is called hierarchy fuzzy process(HFP).Analysis on ambiguous aspects of PDSP under study which is not easy to be defined is prerequisite to evaluate it. HFP is different from algorithm existed in that it clarified the relationship between fuzzy measure and probability measure adopted in AHP and that it directly calculates the family of fuzzy measure from overlapping coefficient and probability measure to treat and evaluate ambiguous and complex aspects of PDSP. A new evaluation algorithm HFP was applied to evaluate level of physical distribution service in the biggest twenty container port in the world. The ranks of the ports are as follows; 1. Rotterdam Port, 2. Hamburg Port, 3. Singapore Port, 4. Seattle Port, 5. Yokohama Port, 6. Long beach Port, 7. Oakland Port, 8. Tokyo Port, 9. Hongkong Port, 10. Kobe Port, 11. Los Angeles Port, 12. New york Port, 13. Antwerp Port, 14. Felixstowe Port, 15. Bremerhaven Port, 16. Le'Havre Port, 17. Kaoshung Port, 18. Killung Port, 19. Bangkok Port, 20. Pusan Port

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Numerical Simulation of Depth-Averaged Flow with a CDG Finite Element Method (CDG 유한요소법을 이용한 수심적분 흐름의 수치모의)

  • Kim, Tae Beom;Choi, Sung-Uk;Min, Kyung Duck
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.26 no.5B
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    • pp.447-457
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    • 2006
  • This paper presents a numerical model for the simulations of 2D depth-averaged flows. The shallow water equations are solved numerically by the Characteristic Dissipative Galerkin (CDG) finite element method. For validation, the developed model is applied to the hydraulic jump. The computed results are compared with the analytical solution, revealing good agreement. In addition, flow in a contracting channel showing standing waves is simulated. The calculated water surface profile appears to be qualitatively consistent with the observed data. The foregoing results indicate that the model is capable of simulating the abrupt change in flow field. Next, the model is applied to the flow in a $180^{\circ}$ curved channel. The simulated results show that the velocity near the inner bank is faster than that near the outer bank and the water depth near the inner bank is shallower than that near the outer bank. However, the simulated results show that the velocity distribution across the channel is almost uniform in the bend except the reach close to the end of the bend. This is due to the limitation of the governing equations in which the transverse convection of momentum by the secondary flows along a channel bend is not taken into account.

Study Analysis of Isocycloseram and Its Metabolites in Agricultural Food Commodities

  • Ji Young Kim;Hyochin Kim;Su Jung Lee;Suji Lim;Gui Hyun Jang;Guiim Moon;Jung Mi Lee
    • Korean Journal of Environmental Agriculture
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    • v.42 no.1
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    • pp.71-81
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    • 2023
  • An accurate and easy-to-use analytical method for determining isocycloseram and its metabolites (SYN549431 and SYN548569) residue is necessary in various food matrixes. Additionally, this method should satisfy domestic and international guidelines (Ministry of Food and Drug Safety and Codex Alimentarius Commission CAC/GL 40). Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) was used to determine the isocycloseram and its metabolites residue in foods. To determine the residue and its metabolites, a sample was extracted with 20 mL of 0.1% formic acid in acetonitrile, 4 g magnesium sulfate anhydrous and 1 g sodium chloride and centrifuged (4,700 G, 10 min, 4℃). To remove the interferences and moisture, d-SPE cartridge was performed before LC-MS/MS analysis with C18 column. To verify the method, a total of five agricultural commodities (hulled rice, potato, soybean, mandarin, and red pepper) were used as a representative group. The matrix-matched calibration curves were confirmed with coefficients of determination (R2) ≥ 0.99 at a calibration range of 0.001-0.05 mg/kg. The limits of detection and quantification were 0.003 and 0.01 mg/kg, respectively. Mean average recoveries were 71.5-109.8% and precision was less than 10% for all five samples. In addition, inter-laboratory validation testing revealed that average recovery was 75.4-107.0% and the coefficient of variation (CV) was below 19.4%. The method is suitable for MFDS, CODEX, and EU guideline for residue analysis. Thus, this method can be useful for determining the residue in various food matrixes in routine analysis.

Quantitative Analysis of Vitamin B5 and B6 Using High Performance Liquid Chromatography (고속액체크로마토그래피를 이용한 비타민 B5 및 B6의 정량 분석)

  • Kim, Gi-Ppeum;Hwang, Young-Sun;Choung, Myoung-Gun
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.46 no.10
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    • pp.1186-1194
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    • 2017
  • Recently, many people have demanded reliable nutritional data even for minor-components. On the other hand, an analytical method for the analyses of vitamin $B_5$ and $B_6$ is lacking. Therefore, this study attempted to validate with accuracy and precision the analysis of vitamin $B_5$ and $B_6$ using a high-performance liquid chromatography (HPLC) method. The vitamin $B_5$ and $B_6$ contents were analyzed using an Agilent 1260 series HPLC system. YMC-Pack ODS-AM ($250{\times}4.6mm$ I.D.) and YMC-Pack Pro RS $C_{18}$ ($250{\times}4.6mm$ I.D.) columns were used for the analyses of vitamin $B_5$ and $B_6$, respectively. In the case of vitamin $B_5$, the flow rate was set to 1.0 mL/min by isocratic elution using the 50 mM $KH_2PO_4$ solution (pH 3.5)/acetonitrile (ACN) (95:5, v/v) with monitoring at 200 nm using HPLC/DAD, whereas the flow rate for vitamin $B_6$ was set to 1.0 mL/min of flow rate by isocratic elution using a 20 mM $CH_3CO_2Na$ solution (pH 3.6)/ACN (97:3, v/v) with monitoring by excitation at 290 nm and emission at 396 nm using HPLC/FLD. The column temperature was set to $30^{\circ}C$. The injection volume was $20{\mu}L$ for each experiment. The specificity of the accuracy and precision for vitamin $B_5$ and $B_6$ were also validated by HPLC. The results showed high linearity in the calibration curve for vitamin $B_5$ ($R^2=0.9998^{{\ast}{\ast}}$), the limit of detection (LOD) and limit of quantitation (LOQ) were 0.4 mg/L and 1.3 mg/L, respectively, In contrast, for the calibration curve of vitamin $B_6$, which showed high linearity ($R^2=0.9999^{{\ast}{\ast}}$), the LOD and LOQ were 0.006 mg/L and 0.02 mg/L, respectively.

Relationship between Job Characteristics and Turnover Intention·Organizational Commitment in EMT(Emergency Medical Technicians) within Medical Institution (의료기관 내 응급구조사의 직무특성과 이직의향 및 조직몰입과의 관련성)

  • Park, Sang-Sub;Park, Jae-Seong
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.14 no.2
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    • pp.768-777
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    • 2013
  • The purpose of this study is to be conducive to work improvement through analyzing turnover intention and organizational commitment of EMT within medical institution. The subjects of this study were randomly extracted 188 EMT. The survey period was conducted from May 3, 2011 to May 19 (May 3rd-4th in G Province, May 14th in B Metropolitan City, May 18th-19th in D Metropolitan City). An analytical method was made with SPSS WIN program(Version 12.0). As a result of research, the turnover intention was high in women(p<.001), in under 30 years old(about 4.9 times, p<.001), in the unmarried(about 4.3 times, p<.001), and in junior college graduate(about 4 times, p<.001). Also, the turnover intention was high in income with under 1,500,000 won(about 3.3 times, p<.001), in working career with under 5 years(about 3.2 times, p<.001), in feeling the legal work limit(about 1.8 times, p<.05), and in group with low job satisfaction(p<.001). In correlation between organizational commitment and job variable, the variables in age, marriage, academic background, turnover intention, income, career, and legal work limit except gender and job satisfaction showed positive correlation with organizational commitment(p<.01). As for the factors affected on the organizational commitment, the turnover intention(p<.01), the legal work limit(p<.01), and the job satisfaction(p<.001) had significant effect on organizational commitment.

Development of a Simultaneous Analytical Method for Azocyclotin, Cyhexatin, and Fenbutatin Oxide Detection in Livestock Products using the LC-MS/MS (LC-MS/MS를 이용한 축산물 중 유기주석계 농약 Azocyclotin, Cyhexatin 및 Fenbutatin oxide의 동시시험법 개발)

  • Nam Young Kim;Eun-Ji Park;So-Ra Park;Jung Mi Lee;Yong Hyun Jung;Hae Jung Yoon
    • Journal of Food Hygiene and Safety
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    • v.38 no.5
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    • pp.361-372
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    • 2023
  • Organotin pesticide is used as an acaricide in agriculture and may contaminate livestock products. This study aims to develop a rapid and straightforward analytical method for detecting organotin pesticides, specifically azocyclotin, cyhexatin, and fenbutatin oxide, in various livestock products, including beef, pork, chicken, egg, and milk, using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The extraction process involved the use of 1% acetic acid in a mixture of acetonitrile and ethyl acetate (1:1). This was followed by the addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium chloride. The extracts were subsequently purified using octadecyl (C18) and primary secondary amine (PSA), after which the supernatant was evaporated. Organotin pesticide recovery ranged from 75.7 to 115.3%, with a coefficient of variation (CV) below 25.3%. The results meet the criteria range of the Codex guidelines (CODEX CAC/GL 40). The analytical method in this study will be invaluable for the analysis of organotin pesticides in livestock products.

Analysis of some pesticides in urine by GC/MS (GC/MS를 이용한 뇨중 몇가지 농약의 분석)

  • Park, Seong-Soo;Park, Song-Ja;Pyo, Hee-Soo;Cho, Jung-Hee;Kim, Hye-Soo;Park, Taek-Kyu
    • The Korean Journal of Pesticide Science
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    • v.4 no.1
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    • pp.1-10
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    • 2000
  • The purpose of this study is to establish the assessment techniques of hazardous chemicals by the development of analytical method of biological samples. In this study, we have developed an extraction method of nine pesticides used for rice paddy that resulted in high recovery from the spiked human urine by the liquid-liquid extraction with diethyl ether at pH 7.0. Calibration curve obtained from each pesticide standard using by gas chromatography/mass spectrometry/selected ion monitoring has shown good linearity and detection limits were the range of $0.4{\sim}2.0$ ng/mL in urine. As a biological monitoring, urine samples of local farmers exposed directly to nine pesticides in the field were collected and analyzed by GC/MS. Of the tested pesticides, metabolites of phenthoate assumed were identified by GC/MS analysis. No parent compound was detected.

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Development of Analytical Method for Sodium Alginate in Foods (식품 중 알긴산나트륨의 분석법 개발)

  • Kim, Hee-Yun;Hong, Ki-Hyoung;Choi, Jang-Duck;Park, Sung-Kwan;Jung, Si-Sub;Choi, Woo-Jeong;Ahn, Yeong-Sun;Hong, Yeong-Pyo;Song, Ok-Ja;Moon, Dong-Chul;Lee, Shin-Ho;Shin, Il-Shik
    • Korean Journal of Food Science and Technology
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    • v.38 no.1
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    • pp.1-4
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    • 2006
  • Method of analyzing sodium alginate in foods was developed using high performance liquid chromatography (HPLC). HPLC conditions for sodium alginate were: column, MCI GEL $(8\;mm\;i.d{\times}300\;mm)$; mobile phase, deionized water; detector, refractive index detection (sensitivity = 16). Separation of sodium alginate was achieved within 15 min. Sodium alginate showed good linear relationship at 0.1-2.0% range. Correlation coefficient of calibration curve for sodium alginate exceeded 0.999, and detection limit was 0.005%. Recovery rate of sodium alginate in wheat flour dough was 106.67%. This method was successfully applied to analyses of cereals, saccharides, and ice cream, etc. Sodium alginate was detected in chocolate, noodles, and kelp at 0-44.8% range.