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Development and Validation of an Analytical Method for Quinoxyfen in Agricultural Products using QuEChERS and LC-MS/MS (QuEChERS법 및 LC-MS/MS를 이용한 농산물 중 살균제 Quinoxyfen의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Choi, Young-Nae;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.140-147
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    • 2019
  • An analytical method was developed for the determination of quinoxyfen in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with 1% acetic acid in acetonitrile and water was removed by liquid-liquid partitioning with $MgSO_4$ (anhydrous magnesium sulfate) and sodium acetate. Dispersive solid-phase extraction (d-SPE) cleanup was carried out using $MgSO_4$, PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed by using LC-MS/MS in positive mode with MRM (multiple reaction monitoring). The matrix-matched calibration curves were constructed using six levels ($0.001-0.25{\mu}g/mL$) and the coefficient of determination ($R^2$) was above 0.99. Recovery results at three concentrations (LOQ, 10 LOQ, and 50 LOQ, n=5) were in the range of 73.5-86.7% with RSDs (relative standard deviations) of less than 8.9%. For inter-laboratory validation, the average recovery was 77.2-95.4% and the CV (coefficient of variation) was below 14.5%. All results were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for quinoxyfen determination in agricultural commodities. This study could be useful for the safe management of quinoxyfen residues in agricultural products.

Optimization for Removal of Nitrogen Using Non-consumable Anode Electrodes (비소모성 Anode(산화전극)을 이용한 질소 제거 최적화)

  • Hyunsang, Kim;Younghee, Kim
    • Clean Technology
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    • v.28 no.4
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    • pp.309-315
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    • 2022
  • Research was conducted to derive the optimal operation conditions and the optimal cathode for using a DSA electrode as an anode to minimize electrode consumption during the removal of nitrogen from wastewater by the electro-chemical method. Of the various electrodes tested as cathodes, brass was determined to be the optimal electrode. It had the highest NO3-N removal rate and the lowest concentration of residual NH3-N, a by-product when Cl is present in the solution. Investigating the effect of current density found that when the initial concentration of NO3-N was 50 mg L-1, the optimal current density was 15 mA cm-2. In addition, current densities above 15 mA cm-2 did not significantly affect the NO3-N removal rate. The effect of electrolytes on removing NO3-N and minimizing NH3-N was investigated by using Na2SO4 and NaCl as electrolytes and varying the reaction times. When Na2SO4 and NaCl are mixed at a ratio of 1.0 g L-1 to 0.5 g L-1 and reacted for 90 min at a current density of 15 mA cm-2 and an initial NO3-N concentration of 50 mg L-1, the removal rate of NO3-N was about 48% and there was no residual NH3-N. On the other hand, when using only 1.5 g L-1 of NaCl as an electrolyte, the removal rate of NO3-N was the highest at about 55% and there was no residual NH3-N.

Synthesis and Structural Study of Extraframework ZrI6Tl119+ Cationic Cluster in Zeolite A (제올라이트 A 동공 내 비골격 ZrI6Tl119+ 양이온 클러스터의 합성과 구조 연구)

  • Hyeon Seung, Lim;Jong Sam, Park;Cheol Woong, Kim;Woo Taik, Lim
    • Korean Journal of Mineralogy and Petrology
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    • v.35 no.4
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    • pp.447-455
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    • 2022
  • Fully dehydrated Tl12-LTA (|Tl12|[Si12Al12O48]-LTA,Tl12-A) was treated with 6.0×103 Pa of ZrI4 (g) at 623 K for 72 hr under anhydrous conditions. The crystal structure of product, |Zr0.25I1.5Tl12|[Si12Al12O48]-LTA, was determined by single-crystal crystallography using synchrotron X-radiation in the cubic space group Pm3m (a = 12.337(2) Å). It was refined using all data to the final error index (for the 712 unique reflections for which Fo> 4σ(Fo) R1/wR2= 0.055/0.189. In this structure, octahedral ZrI62- ions center about 25% of the large cavities (Zr-I = 2.91(4) Å). Each coordinates to eight Tl+ ions and they are further bridged by Tl+ ions in the planes of 8-rings to form a cubic three-dimensional ZrI6Tl119+ cationic cluster. About 1.5 Tl+ ions per unit cell moved to deeper side of sodalite cavity after reaction with ZrI4(g). The remaining Tl+ ions occupy well-established cation positions near 6- and 8-rings.

Voltammetric Sensor Incorporated with Conductive Polymer, Tyrosinase, and Ionic Liquid Electrolyte for Bisphenol F (전도성고분자, 티로시나아제 효소 및 이온성 액체 전해질을 융합한 전압전류법 기반의 비스페놀F 검출 센서)

  • Sung Eun Ji;Sang Hyuk Lee;Hye Jin Lee
    • Applied Chemistry for Engineering
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    • v.34 no.3
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    • pp.258-263
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    • 2023
  • In this study, conductive polymers and the enzyme tyrosinase (Tyr) were deposited on the surface of a screen printed carbon electrode (SPCE), which can be fabricated as a disposable sensor chip, and applied to the detection of bisphenol F (BPF), an endocrine disruptor with proven links to male diseases and thyroid disorders, using electrochemical methods. On the surface of the SPCE working electrode, which was negatively charged by oxygen plasma treatment, a positively charged conductive polymer, poly(diallyldimethyl ammonium chloride) (PDDA), a negatively charged polymer compound, poly(sodium 4-styrenesulfonate) (PSS), and another layer of PDDA were layered by electrostatic attraction in the order of PDDA, PSS, and finally PDDA. Then, a layer of Tyr, which was negatively charged due to pH adjustment to 7.0, was added to create a PDDA-PSS-PDDA-Tyr sensor for BPF. When the electrode sensor is exposed to a BPF solution, which is the substrate and target analyte, 4,4'-methylenebis(cyclohexa-3,5-diene-1,2-dione) is generated by an oxidation reaction with the Tyr enzyme on the electrode surface. The reduction process of the product at 0.1 V (vs. Ag/AgCl) generating 4,4'-methylenebis(benzene-1,2-diol) was measured using cyclic and differential pulse voltammetries, resulting in a change in the peak current with respect to the concentration of BPF. In addition, we compared the detection performance of BPF using an ionic liquid electrolyte as an alternative to phosphate-buffered saline, which has been used in many previous sensing studies. Furthermore, the selectivity of bisphenol S, which acts as an interfering substance with a similar structure to BPF, was investigated. Finally, we demonstrated the practical applicability of the sensor by applying it to analyze the concentration of BPF in real samples prepared in the laboratory.

Effect of Service Convenience on the Relationship Performance in B2B Markets: Mediating Effect of Relationship Factors (B2B 시장에서의 서비스 편의성이 관계성과에 미치는 영향 : 관계적 요인의 매개효과 분석)

  • Han, Sang-Lin;Lee, Seong-Ho
    • Journal of Distribution Research
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    • v.16 no.4
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    • pp.65-93
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    • 2011
  • As relationship between buyer and seller has been brought closer and long-term relationship has been more important in B2B markets, the importance of service and service convenience increases as well as product. In homogeneous markets, where service offerings are similar and therefore not key competitive differentiator, providing greater convenience may enable a competitive advantage. Service convenience, as conceptualized by Berry et al. (2002), is defined as the consumers' time and effort perceptions related to buying or using a service. For this reason, B2B customers are interested in how fast the service is provided and how much save non-monetary cost like time or effort by the service convenience along with service quality. Therefore, this study attempts to investigate the impact of service convenience on relationship factors such as relationship satisfaction, relationship commitment, and relationship performance. The purpose of this study is to find out whether service convenience can be a new antecedent of relationship quality and relationship performance. In addition, this study tries to examine how five-dimensional service convenience constructs (decision convenience, access convenience, transaction convenience, benefit convenience, post-benefit convenience) affect customers' relationship satisfaction, relationship commitment, and relationship performance. The service convenience comprises five fundamental components - decision convenience (the perceived time and effort costs associated with service purchase or use decisions), access convenience(the perceived time and effort costs associated with initiating service delivery), transaction convenience(the perceived time and effort costs associated with finalizing the transaction), benefit convenience(the perceived time and effort costs associated with experiencing the core benefits of the offering) and post-benefit convenience (the perceived time and effort costs associated with reestablishing subsequent contact with the firm). Earlier studies of perceived service convenience in the industrial market are none. The conventional studies that have dealt with service convenience have usually been made in the consumer market, or they have dealt with convenience aspects in the service process. This service convenience measure for consumer market can be useful tool to estimate service quality in B2B market. The conceptualization developed by Berry et al. (2002) reflects a multistage, experiential consumption process in which evaluations of convenience vary at each stage. For this reason, the service convenience measure is good for B2B service environment which has complex processes and various types. Especially when categorizing B2B service as sequential stage of service delivery like Kumar and Kumar (2004), the Berry's service convenience measure which reflect sequential flow of service deliveries suitable to establish B2B service convenience. For this study, data were gathered from respondents who often buy business service and analyzed by structural equation modeling. The sample size in the present study is 119. Composite reliability values and average variance extracted values were examined for each variable to have reliability. We determine whether the measurement model supports the convergent validity by CFA, and discriminant validity was assessed by examining the correlation matrix of the constructs. For each pair of constructs, the square root of the average variance extracted exceeded their correlations, thus supporting the discriminant validity of the constructs. Hypotheses were tested using the Smart PLS 2.0 and we calculated the PLS path values and followed with a bootstrap re-sampling method to test the hypotheses. Among the five dimensional service convenience constructs, four constructs (decision convenience, transaction convenience, benefit convenience, post-benefit convenience) affected customers' positive relationship satisfaction, relationship commitment, and relationship performance. This result means that service convenience is important cue to improve relationship between buyer and seller. One of the five service convenience dimensions, access convenience, does not affect relationship quality and performance, which implies that the dimension of service convenience is not important factor of cumulative satisfaction. The Cumulative satisfaction can be distinguished from transaction-specific customer satisfaction, which is an immediate post-purchase evaluative judgment or an affective reaction to the most recent transactional experience with the firm. Because access convenience minimizes the physical effort associated with initiating an exchange, the effect on relationship satisfaction similar to cumulative satisfaction may be relatively low in terms of importance than transaction-specific customer satisfaction. Also, B2B firms focus on service quality, price, benefit, follow-up service and so on than convenience of time or place in service because it is relatively difficult to change existing transaction partners in B2B market compared to consumer market. In addition, this study using partial least squares methods reveals that customers' satisfaction and commitment toward relationship has mediating role between the service convenience and relationship performance. The result shows that management and investment to improve service convenience make customers' positive relationship satisfaction, and then the positive relationship satisfaction can enhance the relationship commitment and relationship performance. And to conclude, service convenience management is an important part of successful relationship performance management, and the service convenience is an important antecedent of relationship between buyer and seller such as the relationship commitment and relationship performance. Therefore, it has more important to improve relationship performance that service providers enhance service convenience although competitive service development or service quality improvement is important. Given the pressure to provide increased convenience, it is not surprising that organizations have made significant investments in enhancing the convenience aspect of their product and service offering.

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Studies on Glycolipids in Bacteria -Part II. On the Structure of Glycolipid of Selenomonas ruminantium- (세균(細菌)의 당지질(糖脂質)에 관(關)한 연구(硏究) -제2보(第二報) Selenomonas ruminantium의 당지질(糖脂質)의 구조(構造)-)

  • Kim, Kyo-Chang
    • Applied Biological Chemistry
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    • v.17 no.2
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    • pp.125-137
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    • 1974
  • The chemical structure of glycolipid of Selenomonas ruminantium cell wall was to be elucidated. The bacterial cells were treated in hot TCA and the glycolipid fractions were extracted by the solvent $CHCl_3\;:\;CH_3OH$ (1 : 3). The extracted glycolipids fraction was further separated by acetone extraction. The acetone soluble fraction was named as the spot A-compound. The acetone insoluble but ether soluble fraction was named as the spot B-compound. These two compounds were examined for elucidation of their chemical structure. The results were as follows: 1. The IR spectral analysis showed that O-acyl and N-acyl fatty acids were linked to glucosamine moiety in the spot A-compound. However in the spot B-compound in addition to O and N-acyl acids phosphorus was shown to be attached to glucosamine. 2. It was recognized by gas liquid chromatography that spot A compound contained beta-OH $C_{13:0}$ fatty acid in predominance in addition to the fatty acid with beta-OH $C_{9:0}$, whereas the spot B compound was composed of the predominant fatty acid of beta-OH $C_{13:0}$ with small amount of beta-OH $C_{9:0}$. 3. According to the paper chromatographic analysis of hydrazinolysis products of the spot A compound, a compound of a similar Rf value as the chitobiose was recognized, which indicated a structure of two molecules glucosamine condensed. The low Rf value of the hydrazinolysis product of the spot B-compound confirmed the presence of phosphorus attached to glucosamine. 4. The appearance of arabinose resulting from. ninhydrin decomposition of the acid hydrolyzate of the spot A compound indicated that the amino group is attached to $C_2$ of glucosamine. 5. The amount of glucosamine in the N-acetylated spot A compound decreased in half of the original content by the treatment. with $NaBH_4$, indicating that there are two molecules of glucosamines in the spot A compound. The presence of 1, 6-linkage between two molecules of glucosamine was suggested by the Morgan-Elson reaction and confirmed by the periodate decomposition test. 6. By the action of ${\beta}-N-acetyl$ glucosaminidase the N-acetylated spot A compound was completely decomposed into N-acetyl glucosamine, whereas the spot B compound was not. This indicated the spot A compound has a beta-linkage. 7. When phosphodiesterase or phosphomonoesterase acted on $^{32}P-labeled$ spot B compound, $^{32}P$ was not released by phosphodiesterase, but completely released by phosphomonoesterase. This indicated that one phosphorus is linked to glucosamine moiety. 8. The spot A compound is assumed to have the following chemical structure: That is glucosaminyl, ${\beta}-1$, 6-glucosamine to which O-acyl and N-acyl fatty acids are linked, of which the predominant fatty acid is beta-OH $C_{13:0}$ fatty acid in addition to beta-OH $C_{9:0}$ fatty acid 9. The spot B compound is likely to have the linkage of $glucosaminyl-{\beta}-1$, 6-glucosamine to which phosphorus is linked in monoester linkage. Furthermore both O-acyl and N-acyl fatty acids contained beta-OH $C_{13:0}$ fatty acid predominantly in addition to beta-OH $C_{9:0}$ fatty acid.

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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.