• Analytical Science and Technology
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• v.10 no.1
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• pp.9-17
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• 1997

Nitrophenols are a group of important priority pollutants classified by the US Environmental Protection Agency. Reverse-phase liquid chromatographic method combined with mass spectromethy employing atmospheric pressure chemical ionization(APCI) interface is utilized to determine a mixture of nitrophenols in water matrix without any pretreatment. The sensitivity and selectivity for the identification of different kind of nitrophenols is enhanced by the use of selected ion monitoring and cone voltage fragmentation. The fragmentation patterns of nitrophenols are compared with those obtained from the collision induced dissociation(CID) MS/MS technique.

• Analytical Science and Technology
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• v.23 no.6
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• pp.524-530
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• 2010

Chloramphenicol is one of the most effective antibiotics for treatment of food-producing animals for typhoid fever. However, it has been reported that it caused severe side effects such as aplastic anemia in human, therefore the use of chloramphenicol for food-producing animal is prohibited by European Union and other countries. In this study, the analytical method using isotope dilution liquid chromatography-mass spectrometry (ID-LC/MS) was established for accurate determination of chloramphenicol in meat. Chloramphenicol was extracted with ethylacetate from porcine and solid phase extraction cartridge was used for enhancing the recovery. The residue of chloramphenicol in porcine was analyzed using the liquid chromatography mass spectrometer (LC/MS) interfaced with electrospray ionization source. Analysis was performed in negative mode with selected reaction mornitoring mode at m/z 321${\rightarrow}$257 of $[M-H]^-$ ${\rightarrow}$ $[M-H-(HCOCl)]^-$ and m/z 326 ${\rightarrow}$ 262 channels for its isotope. The established method was tested using fortified samples at the level of 0.2 1, 10, $25\;{\mu}g$/kg and analytical results agreed with the gravimetrically fortified values within their uncertainties. This method was validated by analyzing a certified reference material, BCR 445, from IRMM (Institute for Reference Materials and Measurement). Our measurement values agreed with the certified value within their uncertainties. The uncertainty of our measured value was much lower than that the certified value from IRMM.

• Analytical Science and Technology
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• v.16 no.1
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• pp.78-81
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• 2003

Peptides separation in high performance liquid chromatography (HPLC) is very important for the analysis of total proteins using mass spectrometry rather than two-dimensional polyacrylamide gel electrophoresis (2D-PAGE). In this study, we investigated the optimal HPLC condition of peptides for the use of mass fingerprinting. As a result of pursuing a combination of solvent additives for HPLC, water and acetonitile containing both 0.1% trifluoroacetic acid and 0.1% acetic acid respectively showed the most efficient resolution and sensitivity.

• Journal of Practical Engineering Education
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• v.14 no.2
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• pp.327-332
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• 2022

This experiment presents a precise analysis method using a mass spectrometer in the biopharmaceutical market, where utility is expanding. Among various techniques for analyzing the protein drug, somatotropin, the peptide fragments through biochemical sample preparation was analyzed by LC-MS/MS characterization. The analysis process was performed by separation analysis using nanoUPLC and MS/MS analysis using Orbitrap. In the case of somatotropin with 21 tryptic peptides, 13 of them were consistent with theoretical predictions within an average of 1 ppm error.

• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.185-194
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• 2015

This study was performed to establish a single residue analytical method for determining fungicide carpropamid residues in various agricultural commodities. Korean cabbage, apple, brown rice and green pepper were selected as representative crops. Samples were homogenized, extracted with acetone and purified by liquid-liquid partition and Florisil column chromatography. Carpropamid residues were analyzed at 220 nm with reversed phase HPLC equipped octylsilyl and octadecylsilyl column and confirmed using mass spectrometry. ILOQ (Instrumental limit of quantitation) of carpropamid was 2 ng and MLOQ (Method LOQ) was 0.02 mg/kg. Mean recoveries from four kinds of crop samples fortified at three levels (MLOQ, 10LOQ, 100LOQ) in triplicate were in the range of 84~112%. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types.

• Analytical Science and Technology
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• v.25 no.1
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• pp.25-32
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• 2012

Isotope dilution mass spectrometry (ID-MS) based on liquid chromatography tandem mass spectrometry (LC/MS/MS) was developed for the accurate determination of sorbic acid in tea-drink. An isotope analogue of sorbic acid, $^{13}C_2$-sorbic acid, was obtained by custom synthesis. MS was operated in the negative mode with selected reaction monitoring (SRM) mode of $[M-H]^-$ ${\rightarrow}$ $[M-CO_2H]^-$ channel at m/z 111 ${\rightarrow}$ 67 for sorbic acid and at m/z 113 ${\rightarrow}$ 68 for its isotope analogue. Chromatographic separation was accomplished with a C18 column and an isocratic mobile phase of 55% of 50 mM ammonium acetate (pH 4.5) and 45% of methanol. Homogeneous reference materials were prepared for validation of this method, including repeatability and reproducibility tests, by fortifying tea-drink with sorbic acid in our laboratory. Repeatability and reproducibility studies showed that the ID-LC/MS method is a reliable and reproducible method which provides less than 3.8% of relative standard deviation (RSD) for the analysis of sorbic acid.

• The Korean Journal of Pesticide Science
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• v.21 no.1
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• pp.75-83
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• 2017

The single residue analytical method was developed for determining fungicide pencycuron residues in various agricultural commodities with high-performance liquid chromatography (HPLC). Pencycuron residue was extracted with acetone from representative crops such as Korean cabbage, apple, brown rice and green pepper. After ethyl acetate/n-hexane partition and subsequent clean-up with silica gel chromatography, pencycuron residue was quantified by reversed phase HPLC with UV detection at 240 nm. The suspected residue of pencycuron was confirmed using selected-ion monitoring (SIM) LC/mass spectrometry (MS). Instrumental limit of quantitation (ILOQ) and method LOQ (MLOQ) were set at 2 ng and 0.02 mg/kg, respectively. Overall recoveries of pencycuron from different crop samples fortified at three levels (MLOQ, 10MLOQ, 100MLOQ) were 72~108%. This proposed method could be useful as official analytical method for quantification of pencycuron residues in agricultural commodities.

• Korean Journal of Environmental Agriculture
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• v.30 no.3
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• pp.288-294
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• 2011

BACKGROUND: Methylmercury is analyzed by HPLC-ICP/MS because of the simplicity for sample preparation and interference. However, most of the pre-treatment methods for methylmercury need a further pH adjustment of the extracted solution and removal of organic matter for HPLC. The purpose of this study was to establish a rapid and accurate analytical method for determination of methylmercury in fish by using HPLC-ICP/MS. METHOD AND RESULTS: We conducted an experiment for pre-treatment and instrument conditions and analytical method verification. Pre-treatment condition was established with aqueous 1% L-cysteine HCl and heated at $60^{\circ}C$ in microwave for 20 min. Methylmercury in $50{\mu}L$ of filtered extract was separated by a C18 column and aqueous 0.1% L-cysteine HCl + 0.1% L-cysteine mobile phase at $25^{\circ}C$. The presence of cysteine in mobile phase and sample solution was essential to eliminate adsorption, peak tailing and memory effect problems. Correlation coefficient($r^2$) for the linearity was 0.9998. The limits of detection and quantitation for this method were 0.15 and $0.45{\mu}g/kg$ respectively. CONCLUSION: Result for analytical method verification, accuracy and repeatability of the analytes were in good agreement with the certified reference materials values of methylmercury at a 95% confidence level. The advantage of the established method is that the extracted solution can be directly injected into the HPLC column without additional processes and the memory effect of mercury in the ICP-MS can be eliminated.

• Journal of Life Science
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• v.29 no.2
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• pp.198-201
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• 2019

Recently, it has been reported that Bacillus mojavensis possesses antifungal properties and plant growth-promoting activities, which are similar to the characteristics of siderophore. In this study, the siderophore produced by B. mojavensis was assessed using a solid phase extraction (SPE) cartridge and liquid chromatography quadrupole time-of-flight tandem mass spectrometry (Q-TOF MS/MS). After B. mojavensis was incubated in phenol medium for 16 hr and lyophilized, the sample was dissolved in water and loaded to an SPE cartridge to remove interferences. The cartridge was washed with 5% methanol in water and eluted with 2% formic acid in methanol sequentially. The eluted solution was evaporated under a stream of nitrogen gas and reconstituted in methanol. The reconstituted sample was filtered, and $1{\mu}l$ of the sample was assessed using Q-TOF MS/MS. The mass spectrometer was operated using the positive electrospray ionization mode. Based on the mass spectrum and tandem mass spectrum, the siderophore produced by B. mojavensis was bacillibactin, one of the catechol types of siderophore with a molecular weight of 882.2556. This siderophore analysis could provide a justification for the study of B. mojavensis as a functional food and for pharmaceutical applications.

• Korean Journal of Pharmacognosy
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• v.49 no.3
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• pp.278-284
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• 2018

Asimina triloba contains many kinds of annonaceous acetogenins known to have toxicity and/or activity. In this study, analysis of acetogenins was carried out on the extract and its solvent fractions of A. triloba leaves using a liquid chromatography mass spectroscopy(LC-MS). In the extract, the ethanolic extract was significantly higher acetogenin contents than hot water extract. In the analysis of solvent fraction from the ethanolic extract, n-hexane, ethylacetate, and aqueous fraction were contained 85.17~90.92%, 8.96~14.52% and 0.12~0.35% of total acetogenin in the extract. Based on these results, the analytical method is useful for comparing annonaceous acetogenins contents in plant samples. Moreover, when research or product development aiming at the physiological activity of acetogenin such as anticancer activity using A. triloba leaves is performed, a fractionation using a nonpolar organic solvents and alcohol extract may be useful methods. This method can also be used for the purpose of eliminating toxicity as well.