• Journal of Pharmaceutical Investigation
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• v.20 no.2
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• pp.73-78
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• 1990

A sensitive fluorometric method using 9-fluorenylmethyl pentafluorophenyl carbonate (FMPC) as the fluorescent labeling agent was developed to determine D-penicillamine (D-PA). The fluorophore had excitation and emission wavelengths of 260 nm and 313 nm, respectively. After derivatization, the fluorescent product was separated, and quantified by spectrofluorometry. The derivative was highly fluorescent and stable. Optimum condition for the reaction was investigated. A linear response was obtained over the range of $4.0{\times}10^{-7}-5.0{\times}10{-6}\;M$ with the correlation coefficient of 0.999 (n=6). The procedure described was successfully applied to the determination of the dosage forms of capsule with the recovery of $98.62{\pm}0.57%$ (150 mg), $98.36{\pm}0.57%$, (250 mg).

• Journal of Environmental Science International
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• v.4 no.3
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• pp.97-97
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• 1995

PCBs have been measured using GC-ECD, GC-MS, GC-ELCD, HPLC, TLC, NMR and Immunoassay. The analysis of PCBs using GC-ECD include the peak pattern method as none derivatization and the Perchlorination method as derivatization. This study was conducted to establish the perchlorination method with Sbcls from PCBs to decachlorinated biphenyl(DCB). The aroclor 1242 of PCBs was chlorinated and then, converted into the DCB which showed a single peak in GC-ECD chromatogram. The detection limit of DCB was 2pg. The quantification detection concentration of PCBs extracted with soxhlet was 0.5ng/g in the soil. PCBs were not detected in the suburban soil, but 174ng/g in the soil of industrial complex. Mean PCBs concentration of Shinchun stream at Kumho river and Jinchun stream at Nakdong river was calculated average 낙ngjg in 각e sediment. PCBs concentration in the sediment of Kumho river near 2-7km from conjunction with Nakdong river was average 154ng/g. PCBs concentration in the sediment of Nakdong river near conjunction with Kumho river was average 159ng/g.

• Journal of Environmental Science International
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• v.4 no.3
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• pp.249-258
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• 1995

PCBs have been measured using GC-ECD, GC-MS, GC-ELCD, HPLC, TLC, NMR and Immunoassay. The analysis of PCBs using GC-ECD include the peak pattern method as none derivatization and the Perchlorination method as derivatization. This study was conducted to establish the perchlorination method with Sbcls from PCBs to decachlorinated biphenyl(DCB). The aroclor 1242 of PCBs was chlorinated and then, converted into the DCB which showed a single peak in GC-ECD chromatogram. The detection limit of DCB was 2pg. The quantification detection concentration of PCBs extracted with soxhlet was 0.5ng/g in the soil. PCBs were not detected in the suburban soil, but 174ng/g in the soil of industrial complex. Mean PCBs concentration of Shinchun stream at Kumho river and Jinchun stream at Nakdong river was calculated average 낙ngjg in 각e sediment. PCBs concentration in the sediment of Kumho river near 2-7km from conjunction with Nakdong river was average 154ng/g. PCBs concentration in the sediment of Nakdong river near conjunction with Kumho river was average 159ng/g.

• The Korean Journal of Physiology and Pharmacology
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• v.16 no.5
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• pp.355-360
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• 2012

A simple, sensitive and reproducible high-performance liquid chromatography (HPLC) method has been validated for determining concentrations of glutamate, glycine, and alanine in human plasma. Proteins in plasma were precipitated with perchloric acid, followed by derivatization with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC). Simultaneous analysis of glutamate, glycine, and alanine is achieved using reversed-phase HPLC conditions and ultraviolet detection. Excellent linearity was observed for these three amino acids over their concentration ranges with correlation coefficients (r)>0.999. The intra- and inter-day precision were below 10%. This method utilizes quality control samples and demonstrates excellent plasma recovery and accuracy. The developed method has been successfully applied to measure plasma glutamate, glycine, and alanine in twenty volunteers.

• Analytical Science and Technology
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• v.12 no.6
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• pp.571-576
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• 1999

Screening method for NSAIDs (Hon-Steroidal Anti-Inflammatory Drugs) in urine was developed using GC/NCI-MS. Derivatized six fenamates with pentafluoropropionic anhydride showed high sensitivity in NCI-MS. The conditions of the derivatization reaction and chromatographic conditions were established for screening with a trace analysis. Limit of detection was in the range of 4-25 pg/mL. This method may be used to the equine doping analysis for NSAIDs and forensic analysis.

• Archives of Pharmacal Research
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• v.20 no.2
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• pp.184-190
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• 1997

A new method based on the chemical reaction has been devised for the sequential analysis of reducing oligosaccharides using 8-amino-2-naphthalenesulfonic acid (ANS), a fluorescent precolumn derivatization reagent for reducing saccharides. The procedure established includes 1) the derivatization of a reducing oligosaccharide to produce a Schiff base, 2) the reduction of the base with sodium cyanoborohydride $(NaBH_3/CN), 3)$ the methoxycarbonylation of the resultant secondary amino group, 4) the cleavage of the glycoside bond next to the reducing end, based on the intramolecular acid hydrolysis by the action of a sulfonic acid group of the ANS derivative, 5) the identification of the liberated reducing end by high-performance liquid chromatography (HPLC), and finally 6) the recovery of the resultant oligosaccharide fragment from the cleavage reaction mixture. The extensive examination of the conditions for the sequential analysis of reducing oligosaccharides resulted in the procedure of simplicity , high selectivity and high recovery. This procedure was found to be useful for the sequential analysis of di-, tri- and tetrasaccharides.

• Mass Spectrometry Letters
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• v.13 no.4
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• pp.133-138
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• 2022

Taurine is a type of sulfur-containing amino acid having a sulfate functional group, that is biosynthesized from cysteine. It is mainly distributed in high concentrations in animal tissues and is known to have various effects such as osmotic pressure control, calcium control, anti-inflammatory, antioxidant, and hepatocellular protection. Also, taurine deficiency causes a variety of symptoms, including visual impairment. In particular, in the case of cats, taurine is not biosynthesized and must be supplied through food, so it is classified as an essential amino acid. In this study, an analysis method using mass spectrometry was developed instead of the commonly used derivatization method to quickly, environmentally, and precisely analyze taurine in various animal feeds. The developed analytical method showed good linearity (R² > 0.99), accuracy (81.97-105.78%), and precision (0.07-12.37%). In addition, the developed method was further verified through quantitative comparison with the derivatization method. This developed method was used in the determination of taurine in 20 animal feed samples obtained from South Korea. The levels of taurine found ranged from 81.53 to 6,743.53 mg/kg. The developed analysis method will be used for the detection and quantification of taurine in domestic feed.

• KSBB Journal
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• v.30 no.5
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• pp.230-238
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• 2015

Abnormal glycosylation can significantly affect the intrinsic functions (i.e., stability and solubility) of proteins and the extrinsic protein interactions with other biomolecules. For example, recombinant glycoprotein therapeutics needs proper glycosylation for optimal drug efficacy. Therefore, there has been a strong demand for rapid, sensitive and high-through-put glycomics tools for real-time monitoring and fast validation of the biotherapeutics glycosylation. Although liquid chromatography tandem mass spectrometry (LC-MS/MS) is one of the most powerful tools for the characterization of glycan structures, it is generally time consuming and requires highly skilled personnel to collect the data and analyze the results. Recently, as an alternative method, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-MS), which is a fast, robust and easy-to-use instrumentation, has been used for quantitative glycomics with various chemical derivatization techniques. In this review, we highlight the recent advances in MALDI-MS based quantitative glycan analysis according to the chemical derivatization strategies. Moreover, we address the application of MALDI-MS for high-throughput glycan analysis in many fields of clinical and biochemical engineering.

• Journal of Pharmacopuncture
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• v.18 no.1
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• pp.44-55
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• 2015

Objectives: Scolopendra subspinipes mutilans (S. subspinipes mutilans) is known as a traditional medicine and includes various amino acids, peptides and proteins. The amino acids in the pharmacopuncture extracted from S. subspinipes mutilans by using derivatization methods were analyzed quantitatively and qualitatively by using high performance liquid chromatography (HPLC) over a 12 month period to confirm its stability. Methods: Amino acids of pharmacopuncture extracted from S. subspinipes mutilans were derived by using O-phthaldialdehyde (OPA) & 9-fluorenyl methoxy carbonyl chloride (FMOC) reagent and were analyzed using HPLC. The amino acids were detected by using a diode array detector (DAD) and a fluorescence detector (FLD) to compare a mixed amino acid standard (STD) to the pharmacopuncture from centipedes. The stability tests on the pharmacopuncture from centipedes were done using HPLC for three conditions: a room temperature test chamber, an acceleration test chamber, and a cold test chamber. Results: The pharmacopuncture from centipedes was prepared by using the method of the Korean Pharmacopuncture Institute (KPI) and through quantitative analyses was shown to contain 9 amino acids of the 16 amino acids in the mixed amino acid STD. The amounts of the amino acids in the pharmacopuncture from centipedes were 34.37 ppm of aspartate, 123.72 ppm of arginine, 170.63 ppm of alanine, 59.55 ppm of leucine and 57 ppm of lysine. The relative standard deviation (RSD %) results for the pharmacopuncture from centipedes had a maximum value of 14.95% and minimum value of 1.795% on the room temperature test chamber, the acceleration test chamber and the cold test chamber stability tests. Conclusion: Stability tests on and quantitative and qualitative analyses of the amino acids in the pharmacopuncture extracted from centipedes by using derivatization methods were performed by using HPLC. Through research, we hope to determine the relationship between time and the concentrations of the amino acids in the pharmacopuncture extracted from centipedes.

• Applied Biological Chemistry
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• v.40 no.5
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• pp.442-446
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• 1997

A new analytical method was developed by HPLC after supercritical fluid extraction and fluorogenic derivatization for the determination of quinclorac (3,7-dichloro-8-quinoline carboxylic acid) in soil. The graminicide quinclorac was extracted from soil by supercritical fluid extraction. Supercritical carbon dioxide at 7000 psi $(80^{\circ}C)$ modified with 30% of methanol extracted quinclorac from soil samples at the level of $0.1ng\;g^{-1}$ with 96% recovery. Extracted quinclorac was determined by HPLC as a fluorescent derivative. Derivatization was made with 4-bromomethyl-7-methoxycoumarin (4-Br-Mmc) using 18-crown-6-ether as a catalyst. The conversion was completed within 30 min and the limit of detection was 0.5 ppb to prove that the procedure could be used in the residue analysis of the pesticides containing carboxylic acid group.