• Proceedings of the PSK Conference
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• 2003.10b
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• pp.241.3-242
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• 2003

A simple, specific and sensitive method for the determination of methyltestosterone (MT) in human serum has been developed by gas chromatography/mass spectrometry with the purpose of conducting pharmacokinetic and bioequivalence studies of MT. This method involves the use of liquid-liquid extraction with diethyl ether and derivatization with MSTFA, using 1 ml of serum obtained from volunteers orally taken 50 mg MT. MT showed good resolutions in this conditions and no significant interfering peaks were observed. (omitted)

• Bulletin of the Korean Chemical Society
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• v.34 no.6
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• pp.1783-1790
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• 2013

A simultaneous analytical method has been developed for the fluorimetric determination of haloacetonitriles (HANs) [dichloroacetonitrile (DCAN), trichloroacetonitrile (TCAN), dibromoacetonitrile (DBAN), haloacetamides [dichloroacetamide (DCAD), and trichloroacetamde (TCAD)] in drinking water by using the combined on-line perconcentration/reversed phase liquid chromatography (RPLC)-postcolumn detection system. This on-line perconcentration system was achieved by employing a precolumn packed with a commercial solid phase extraction (SPE) sorbent for the enrichment and purification of the target analytes. The haloacetonitriles and haloacetamides were separated on CN analytical column in a 7.5% methanol-0.02 M phosphate buffered mobile phase at pH 3. The column effluents were reacted with postcolumn reagents of ophthaldialdehyde (OPA) and sulfite ion at pH 11.5, to produce a highly fluorescent isoindole fluorophore, which were measured with a fluorescence detector. Under the optimized conditions for RPLC and the postcolumn derivatization system all of the coefficient of determination of the standard calibration curves for the target analytes were over 0.99 and had a linear range from 5 to 100 ${\mu}g/L$. The detection limits showed 1.6 ${\mu}g/L$ for DCAD, 0.1 ${\mu}g/L$ for TCAD, 0.6 ${\mu}g/L$ for DCAN, 1.6 ${\mu}g/L$ for TCAN and 1 ${\mu}g/L$ for DBAN, and the recoveries were ranged from 64 to 99% except for DCAD with precisions less than 4.9% in distilled water, and from 72(${\pm}4%$) to 116%(${\pm}2%$) in tap water.

• Tribology and Lubricants
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• v.28 no.6
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• pp.315-320
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• 2012

For proper functioning, general machines usually need lubricant oil as a cooling, cleaning, and sealing agent at points of mechanical contact. The quality of lubricant oil can deteriorate during operation owing to various causes such as high temperature, combustion products and extraneous impurities. In this study, a heavy load stopped during operation, and the oil was analyzed to check whether any impurities were added. Extraction using acetonitrile followed by reaction with BSTFA(bistrimethylsilyl trifluoroacetamide) showed that, trimethylsilylated ethylene glycol was present in the lubricant oil. To quantify the ethylene glycol in the oil, deuterium-substituted ethylene glycol, which acted as an internal standard, was added to the sample and then extracted with the solvent. Next, the extract was reacted with the derivatizing agent(BSTFA) and then analyzed with GC/MS. The detection limit of this method was found to be $0.5{\mu}g/g$ and the recovery of oil containing $20,000{\mu}g/g$ of ethylene glycol was measured to be 94.8%. A damaged O-ring and eroded cylinder liner were found during the overhaul, which implied the leakage of coolant containing ethylene glycol into the lubricating system. The erosion of the cylinder liner was assumed to be due to cavitation of the coolant in the cooling system.

• YAKHAK HOEJI
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• v.20 no.3
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• pp.125-129
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• 1976

The aim of this investigation was to develop a quantitative gas-liquid chromatographic method of analysis forhyosyamine and scopolamine, and to apply this method to the analysis of preparations. The trimethylsily(TMS) derivatives of the alkaloids were found to be far superior to the nonsilylating compounds in charomatagrams. Bis(trimethylsilyl) acetamide(BSA) was evaluated and found to be a good reagent for silyation of the alkaloids. The optimum derivatization conditions were heating the alkaloids in a closed tube at $70^{\circ)$ for 30 min with a 150 molar excess of BSA to the alkaloids were found to be alkaloids. Calibration curves for the two alkaloids were alkaloid. The standard deviations were 1.1% for hyoscyamine and 1.5% for scopolamine. The minimum detectable amount using the hydrogen flame ionization edtector was determined to be 2$\times$10$^{-11}$ moles of each alkaloid injected.

• Archives of Pharmacal Research
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• v.17 no.5
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• pp.337-342
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• 1994

Carbohydrate analysis is important in studying structure and activity of complex polysaccharides. New analytical method was applied to get an information on the composition of polysaccharides showing antitumor activity. Monosaccharides were labeled with 7-amino-1, 3-naph-thalenedisulfonic acid (7-AGA) by reductive amination and separated by HPLC. Five kinds of polysaccharides from Basidiomycetes were hydrolyzed and analyzed in combination with electrophresis and HPLC. At the same time, alditol acetate derivatives were prepared and analyzed by gas chromatography. Two different techniques using different derivatization methods showed very similar results. The monosaccharides from Coriolus versicolor and Cordyceps militaris were glucose and galactose. Phellinus linteus composed of glucose, glactose, mannose, arabinose and fucose. The HPLC method with fluorescence detector was very sensitive compared to other methods.

• Journal of Integrative Natural Science
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• v.8 no.2
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• pp.111-116
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• 2015

Liquid chromatographic enantiomer separation of ${\alpha}$-amino acid esters as nitrobenzoxadiazole (NBD) derivatives was performed using several chiral stationary phases (CSPs) based on polysaccharide derivatives under fluorescence detection. For enantiomer separation by normal HPLC, the non-aqueous derivatization method of ${\alpha}$-amino acid esters for NBD analytes was introduced. Among the six CSPs used in this study, the performance of Chiralpak IA was superior for enantiomer resolution of NBD derivatives of several ${\alpha}$-amino acid methyl esters. Also the convenient analytical method using polysaccharide-derived CSPs developed in this study was applied to determine the optical purity of ${\alpha}$-amino acids esters. It was investigated that the enantiomeric impurity levels of 0.02-1.73% were found after determination of enantiomeric purities of several commercially available L-amino acid methyl esters. It is expected to be quite useful for enantiomer separation of other ${\alpha}$-amino acid esters as NBD derivatives by normal HPLC.

• Analytical Science and Technology
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• v.17 no.6
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• pp.527-531
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• 2004

Treatment with aqueous sodium hydroxide solution plays an important role to impart certain desirable properties - feel and luster on the surface of polyester fiber. In this process alkali wastewater contains disodium terephthalate, ethylene glycol (EG) and residual sodium hydroxide. In this paper we report a new method containing the pretreatments of derivatization with benzoyl chloride and solvent extraction using pentane. The calibration curve of EG determined by GC/MS-SIM shows a good linearity in the range of 0.1 to $25{\mu}g/mL$ having the standard deviation of ${\leq}8.7%$. The recovery and the detection limit of this method are 91.9-93.7% and $0.05{\mu}g/mL$ respectively.

• YAKHAK HOEJI
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• v.41 no.4
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• pp.414-420
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• 1997

A rapid and sensitive high performance liquid chromatographic method with UV detection for the analysis of polyamines(putrescine, spermidine, spermine) has been developed. The benzoyl chloride derivatives of putrescine, spermidine and spermine are separated on a mc-Bondapak C18 reverse-phase column with 50% methanol as the mobile phase. This method was applied to the analysis of polyamines in the serum of normal human and uterine cancer patients. The results show that the mean level of polyamines in cancer patients serum is much higher than that in normal human serum.

• Analytical Science and Technology
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• v.36 no.5
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• pp.224-235
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• 2023

An analytical method was developed for the determination of phenol (P) and the seven substituted phenols in water samples and fish tissue samples collected from three streams located in eastern Gangwon State in spring and summer. The phenols were extracted and then derivatized to phenyl acetates using acetic anhydride. The derivatives were subsequently identified and quantified using gas chromatography coupled with mass spectrometry. P and 4-nitrophenol (4NP) were found at relatively high levels in water, ranging from below the method detection limit (MDL) to 3.32 ㎍/L and from < MDL to 4.91 ㎍/L, respectively. P and 4NP were also the dominant compounds in the fish tissue, ranging from < MDL to 407 ㎍/kg and from < MDL to 870 ㎍/kg, respectively. Phenol concentrations were significantly higher in spring than in summer. The ecological risk quotient calculated for P was higher than 4NP but not high enough to pose any risk of adverse effects to fish health.

• Analytical Science and Technology
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• v.12 no.5
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• pp.408-414
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• 1999

A selective and sensitive method for the derivatization of total homocysteine (Hcy) and the related compounds in plasma by gas chromatograph (GC)-electron capture detector (ECD) has been developed. To determine total homocysteine, cysteine (Cys), and methionine (Met) in human plasma using GC-ECD, analytes were reduced and converted into their N(O,S)-ethylearbonyl pentafluoropropyl (PFP) ester by derivatization with ethyl chloroformate and pentafluoropropyl alcohol (PFP-OH) in plasma. The best derivatizing agent N(O,S)-ethyl carbonyl PFP ester, was chosen by comparing the sensitivity of derivatized analysis in GC-ECD. The derivatized analytes in plasma were extracted by chloroform, and subsequently back-extracted with hexane and analyzed by GC-ECD. The calibration carves ($R^2$ > 0.990) were linear over the range $5-50{\mu}mol/L$ of Hcy and Met, $40-400{\mu}mol/L$ of Cys spiked in plasma. The detection limit observed by the established method was below $0.5{\mu}mol/L$. This method is highly sensitive and specific in the analysis of Hcy, Cys, and Met. Therefore, we suggest that this method is appropriate in the analysis of trace concentration of Hcy, Cys, and Met in biological fluids.