• Journal of the Korean Chemical Society
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• v.20 no.5
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• pp.351-357
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• 1976

Adsorption isotherms of benzene and p-xylene on both of Spheron 6 (a graphitized carbon black) and Alucer (Alumina) are obtained at various temperatures using a sensitive quartz beam microbalance. From these isotherms BET plots are made to obtain the molecular areas of these adsorbates. On the Spheron 6, the molecular area of p-xylene remains constant until the temperature is increased up to $19^{circ}C$, increases abruptly at $19^{circ}C$ through $19.2^{circ}C$, and then again remains constant thereafter. On the other hand, adsorbed benzene molecules give a quite temperature-independent molecular area. The results are interpreted as the adsorbed p-xylene molecules and benzene molecules are localized on the adsorbents with compact packing, while it gains a hindered-rotational degree of freedom at the expense of vibrational one at the higher temperatures. This peculiar behavior of adsorption is considered as due to the interactions between benzene rings of adsorbents and graphite surface. Molecular areas of these adsorbates on Alucer M. A. increase gradually with temperature, indicating that the adsorbed molecules are unlocalized.

• YAKHAK HOEJI
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• v.57 no.4
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• pp.250-257
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• 2013

Biosimilars are important drugs in medicine and contain many glycosylated proteins. Thorough analysis of the glycosylated protein is a prerequisite for evaluation of biosimilar glycan drugs. A method to assess the diversity of N-glycosylation sites and N-glycans from biosimilar glycan drugs has been developed using two separate methods, LC-MS/MS and MALDI-TOF MS, respectively. Development of sensitive, accurate, and efficient methods for evaluation of glycoproteins is still needed. In this study, analysis of both N-glycosylation sites and N-glycans of glycoprotein was performed using the same LC-MS/MS with two different nano-LC columns, nano-C18 and nano-porous graphitized carbon (nano-PGC) columns. N-glycosylated proteins, including RNAse B (one N-glycosylation site), Fetuin (three sites), and ${\alpha}$-1 acid glycoprotein (four sites), were used, and small amounts of each protein were used for identification of N-glycosylation sites. In addition, high mannose N-glycans (one type of typical glycan structure), Mannose 5 and 9, eluted from RNAse B, were successfully identified using nano-PGC-LC MS/MS analysis, and the abundance of each glycan from the glycoprotein was calculated. This study demonstrated an accurate and efficient method for determination of N-glycosylation sites and N-glycans of glycoproteins based on high sensitive LC-MS/MS using two different nano-columns; this method could be applied for evaluation of the quality of various biosimilar drugs containing N-glycosylation groups.

• Journal of Ginseng Research
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• v.45 no.5
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• pp.539-545
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• 2021

Background: Red ginseng polysaccharides (RGPs) have been acknowledged for their outstanding immunomodulation and anti-tumor activities. However, their studies are still limited by the complexity of their structural features, the absence of purification and enrichment methods, and the rarity of the analytical instruments that apply to the analysis of such macromolecules. Thus, this study is an attempt to establish a new mass spectrometry (MS)-based analysis procedure for RGPs. Methods: Saponin pre-excluded powder of RG (RG-SPEP, 10 mg) was treated with 200 µL of distilled water and centrifuged for 5 h at 1000 rpm and 85 ℃. Ethanol-based precipitation and centrifugation were applied to obtain RGPs from the heated extracts. Further, endo-carbohydrase treatments were performed to produce specific saccharide fragments. Solid-phase extraction (SPE) processes were implemented to purify and enrich the enzyme-treated RGPs, while matrix-assisted laser desorption/ionization time-of-flight/time-of-flight (MALDI-TOF/TOF) MS was employed for the partial structural analysis of the obtained RGPs. Results: Utilizing cellulase, porous graphitized carbon (PGC), hydrophilic interaction chromatography (HILIC), and MALDI-TOF/TOF MS, the neutral and acidic RGPs were qualitatively analyzed. Hex_n and Hex_n-18 (cellulose analogs) were determined to be novel neutral RGPs. Additionally, the [Unknown + Hex_n] species were also determined as new acidic RGPs. Furthermore, HexA_n (H) was determined as another form of the acidic RGPs. Conclusion: Compared to the previous methods of analysis, these unprecedented applications of HILIC-SPE and MALDI-TOF/TOF MS to analyze RGPs proved to be fairly effective for fractionating and detecting neutral and acidic components. This new procedure exhibits great potential as a specific tool for searching and determining various polysaccharides in many herbal medicines.

• Journal of Food Hygiene and Safety
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• v.36 no.3
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• pp.220-227
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• 2021

Fluoroimide is a fungicide and is also used as a pesticide for persimmons and potatoes. The established fluoroimide pesticide analysis method takes a long time to perform and uses benzene, a carcinogen. In addition, a lower limit of quantification is required due to enforcement of the Positive List System. Therefore, this study aimed to improve the analysis method for residual fluoroimide to resolve the problems associated with the current method. The analytical method was improved with reference to the increased stability of fluoroimide under acidic conditions. Fluoroimide was extracted under acidic conditions by hydrogen chloride (4 N) and acetic acid. MgSO₄ and NaCl were used with acetonitrile. C₁₈ (octadecylsilane) 500 mg and graphitized carbon black 40 mg were used in the purification process. The experiment was conducted with agricultural products (hulled rice, potato, soybean, mandarin, green pepper), and liquid chromatograph-tandem mass spectrometry was used for the instrumental analysis. Recovery of fluoroimide was 85.7-106.9% with relative standard deviations (RSDs) of less than 15.6%. This study reports an improved method for the analysis of fluoroimide that might contribute to safety by substituting the use of benzene, a harmful solvent. Furthermore, the use of QuEChERS increased the efficiency of the improved method. Finally, this research confirmed the precise limit of quantification and these results could be used to improve the analysis of other residual pesticides in agricultural products.

• Journal of the Korean Electrochemical Society
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• v.2 no.2
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• pp.75-80
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• 1999

Li-ion cells employ lithium transtion metal oxide as the cathode material and carbon as anode material. To manufacture Li-ion cell with higher capacity and better cycle life, the utilization of electrode materials should be as high as possible without lithium deposition onto the carbon surface during charging. A careful design of cell balance between cathode and anode materials as well as a proper charge method is a key factor to design Li-ion cell with long cycle life. In this study, we investigated the effect of cathode/anode weight ratio on the performance of $LiCoO_2/MPCF$ cell. First we evaluated the charge-discharge behaviours of half-cells. And cylindrical Li-ion cells were fabricated using graphitized MPCF anode and $LiCoO_2$ cathode. The voltage profiles for each half-cell in $LiCoO_2/MPCF$ cell were measured by using lithium metal as a reference electrode. Also, we evaluated the cyclic performance of $LiCoO_2/MPCF$ cells according to weight ratio. From the result of experiment $LiCoO_2$ cathode utilization was independent of weight ratio, but MPCF anode utilization was dependant on weight ratio. Also, the optimal weight ratio of $LiCoO_2/MPCF$ cell was found to be $2.0\~2.2$.

• Journal of Food Hygiene and Safety
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• v.29 no.4
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• pp.285-291
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• 2014

Saflufenacil is a low-volatile and uracil-based herbicide. This herbicide is used for pre-and post-emergence control of major broadleaf weeds. The objective of present study was to develop and validate an analytical method for saflufenacil determination in agricultural products for ensuring the food safety. The saflufenacil residues in samples were extracted with acetone, dichloromethane, and then purified with silica and graphitized carbon cartridge. The purified samples were analyzed by HPLC-UVD and confirmed with LC-MS. The linear range of saflufenacil was $0.1{\sim}5.0{\mu}gmL^{-1}$ with the correlation coefficient (r) = 0.999. Average recoveries of saflufenacil ranged from 80.5% to 110.2% at the spiked level of $0.02{\sim}0.5mgkg^{-1}$, while the relative standard deviation was 0.3~7.3%. In addition, the limit of detection and limit of quantification were 0.005 and $0.02mgL^{-1}$, respectively. Furthermore, an interlaboratory study among three labs was conducted to validate the method, and the results were satisfactory.

• Composites Research
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• v.37 no.3
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• pp.162-169
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• 2024

In this study, PAN(polyacrylonitrile)-based precursor fibers were produced through a wet-spinning process, and their morphologies and graphitization behavior were investigated in the presence of two graphitization catalysts (Ca, Ni). The graphitization catalysts were introduced into the formed pores during hot-water stretching of wet-spun PAN-based precursor fibers. The catalytic effects of graphitization catalysts were examined through crystal structure and Raman analysis. At a relatively low temperature of 1500℃, the graphitization was not significantly affected, whereas at a high temperature of 2400℃, the obtained I_D/I_G value of graphite fiber (GF-Ni100) was decreased by about twice (~0.28) compared to the untreated fibers (GF-AS~0.54). By comparing the I_D/I_G values (GF-Ca100~0.42: GF-Ni100~0.28) of Ca and Ni graphitization catalyst, it was found that the degree of graphitization of Ni graphitization catalyst showed higher influence than that of Ca graphitization catalyst. Moreover, 2D band was also observed, indicating that the graphite plane structures composed of multiple layers were developed. XRD results confirmed that the crystal inter-planar distance (d₀₀₂) of the graphite crystal was slightly decreased after the treatment with the graphitization catalyst, But, the crystal size of Ca-treated graphite fiber (GF-Ca100) was increased by up to ~5 nm.

• 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.

• 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.

• Journal of Food Hygiene and Safety
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• v.34 no.2
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• pp.115-123
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• 2019

An analytical method was developed for the determination of fenpropimorph, a morpholine fungicide, in hulled rice, potato, soybean, mandarin and green pepper using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation and LC-MS/MS (liquid chromatography-tandem mass spectrometry). The QuEChERS extraction was performed with acetonitrile followed by addition of anhydrous magnesium sulfate and sodium chloride. After centrifugation, d-SPE (dispersive solid phase extraction) cleanup was conducted using anhydrous magnesium sulfate, primary secondary amine sorbents and graphitized carbon black. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.0025 to 0.25 mg/kg, and their correlation coefficient ($R^2$) of five agricultural products were higher than 0.9899. The limits of detection (LOD) and quantification (LOQ) were 0.001 and 0.0025 mg/kg, respectively, and the limits of quantification for the analytical method were 0.01 mg/kg. Average recoveries spiked at three levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) and were in the range of 90.9~110.5% with associated relative standard deviation values less than 5.7%. As a result of the inter-laboratory validation, the average recoveries between the two laboratories were 88.6~101.4% and the coefficient of variation was also below 15%. All optimized results were satisfied the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. This study could serve as a reference for safety management relative to fenpropimorph residues in imported and domestic agricultural products.