• The Korean Journal of Food And Nutrition
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• v.9 no.2
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• pp.213-216
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• 1996

A modified method is given for the precolumn derivatization and subsequent high-pressure liquid chromatographic seperation of 3-methylhistidine from urine. The elution contained isocratic solution with acetonirile and 10 M sodium phosphate(pH 7.5) requires less than 7 min. The recoveries of 3-methylhlstidine from urine control were 95% to 106%. 3-Methylhistidine determinations were performed on urine samples from volunteers who were both male trained and non-trained physical undergraduates. As the result, urinary .3-methylhistidine content of volunteers increased significantly after weight training.

• YAKHAK HOEJI
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• v.26 no.2
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• pp.117-121
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• 1982

This investigation was intended to develope the quantitative gas liquid chromatographic method for quercetin. The method involves derivatization of the sample with trimethylsilylimidazole containing cholesterol as an internal standard and injection into a gas chromatograph with 3% OV-17 column. The calibration curve for the quercetin was linear over a sample in the range of 4-16.mu.g. The minimum detectable amount using FID in $1.6{\times}10^{-10}$ a.f.s. was determined to be $6.64{\times}10^{-10}mol$.

• Analytical Science and Technology
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• v.23 no.6
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• pp.551-559
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• 2010

This study was conducted to establish an analytical method for the determination of seven nitrosamines in chlorinated tap water by precolumn derivatization followed by high performance liquid chromatography coupled with fluorescence detection. The derivatization procedure was optimized for denitrosation and dansylation, and then two extraction methods, liquid-liquid extraction (LLE) with dichloromethane and solid phase extraction (SPE), were compared. The SPE method employing the optimized derivation procedure showed higher extraction recovery (54.4-88.7%) and reproducibility (1.9-19.4%) than the LLE method (51.4-87.7% and 4.2-33.3%, respectively). The method detection limits were between 0.5 and 4.4 ng/L. When chlorinated water samples were collected from two treatment plants and ten household taps, and analyzed for nitrosamines, Nnitrosodimethylamine (NDMA) was the major compound found between 26.1 and 112 ng/L.

• The Korean Journal of Pesticide Science
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• v.9 no.2
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• pp.159-165
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• 2005

A sensitive derivatization method by using the TFE/TFAA as derivative reagent is proposed for the determination of acidic herbicides in water, by using this method, method detection limits are improved by 10 times and sample volumes are decreased by 5 times compared with other methods such as U.S. EPA and SPEED 98. And also, in order to suggest higher creditable standard operating procedure (SOP), intra- and inter-lab validation test carried out by four laboratories include our lab. The results of intra and inter-lab validations in same experimental conditions show good linearity in given range of concentrations as a $0.1{\sim}10.0$ ng/ml, and range of accuracies and precisions show $-20.5{\sim}12.2$ bias%, $0.55{\sim}24.48%$ (for intra-lab validation) and $-6.66{\sim}0.80 bias%$, $1.92{\sim}13.86%$ (for inter-lab validation), respectively.

• Analytical Science and Technology
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• v.17 no.4
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• pp.322-336
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• 2004

The improved derivatization technique of tamoxifen metabolite in human urine is described for the acylation method that they are substituted by derivatization reagent like acyl anhydride for use of gas chromatography/mass spectrometry. The hydroxyl group of tamoxifen metabolite was derivatized by trifluoroacetic anhydride (TFAA), pentafluoroacetic anhydride (PFPA) and heptaflorobutylic anhydride (HFBA). It was investigated to the gas chromatography/mass spectrometry (GC/MS) technique use negative ion chemical ionization (NCI), positive ion chemical ionization (PCI) and electron impact (EI). In acylation of the metabolites of tamoxifen, the effective reaction temperature and time were shown to be at $50^{\circ}C$ for 30 min. The 4-hydroxytamoxifen, which is known to major metabolite of tamoxifen, was not detected in human urine, whileas the hydroxymethoxytamoxifen was detected. We thought that this result was from the single dose of tamoxifen.

• Bulletin of the Korean Chemical Society
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• v.34 no.9
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• pp.2787-2794
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• 2013

Cholesterol and cholesterol oxidation products (COPs) may accumulate in foods of animal origin during processing or storage. An effective and sensitive analytical method was developed by increasing the UV absorption of compounds through derivatization by attaching a chromophore to the functional groups of cholesterols (cholesterol, 20-hydroxycholesterol, 7-ketocholesterol, cholestane-$3{\beta}$-$5{\alpha}$-$6{\beta}$-triol, 25-hydroxycholesterol, and $5,6{\alpha}$-epoxycholesterol). The influences of the reaction time, volume of reaction solvent, amounts of derivatizing reagent, and extraction solvents were investigated, as they may influence the reaction and extraction yield. The derivatized COPs were analyzed simultaneously on a C18 column (2.1 mm i.d. ${\times}$ 100 mm length, $3.5{\mu}m$ particle size) using a gradient elution with water and acetonitrile. The derivatized COPs showed increased sensitivity and selectivity in HPLC/UV-Vis. The LOD and LOQ were in the concentration ranges of 0.018-0.55 mg/kg and 0.059-1.84 mg/kg from the powdered milk. And the accuracy and precision were 78.1-116.7% and 1.1-9.9%, respectively.

• Korean Journal of Veterinary Research
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• v.40 no.1
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• pp.35-41
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• 2000

We established a new method to analyze abamectin using HPTLC (high performance thin layer chromatography) in order to obtain its pharmacokinetic profiles in pigs. Recovery of abamectin in pig serum after fluorescence derivatization was $80.01{\pm}3.82%$ at 0.1ppm and $83.67{\pm}3.63%$ at 10ppm, respectively. Detection reproducibility in terms of coefficient variation (c.v.) was 3.09% and 2.74% (intra-day), and 3.71% and 51.7%(inter-day), for 0.1 and 10ppm, respectively. Pharmacokinetics of abamectin was studied in five Yorkshire-Landrace mixed bred male pigs ($35.0{\pm}2.7kg$) administered intramuscularly 0.3mg/kg b.w. Pharmacokinetic profiles of abamectin in pigs were described by the 1-compartment open model with first-order absorption and first-order elimination. AUC (area under the curve) was $262.65{\pm}16.44ng{\cdot}day/ml$ and the biological elimination half-life ($t_{1/2},\;k_e$) was $5.28{\pm}0.84$ days, indicating somewhat high bioavailability and long half-life by the intramuscular route. We suggest intramucular injection of abamectin could be also used in place of the recommended route of its subcutaneous administration so far.

• YAKHAK HOEJI
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• v.37 no.1
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• pp.1-8
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• 1993

A procedure for the high-performance liquid chromatographic determination of Nebramycin factors in fermentation broth of Streptoalloteichus hindustanus ATCC 31218 mutant was investigated using pre-column derivatization and LTV detection. The method is based on pre-column derivatization of Nebramycin factors with 2,4-dinitrofluorobenzene(DNFB) in the presence of Tris (hydroxymethyl)aminoethane. The chromatographic separation of derivatives of Nebramycin factors and unknown impurities is achieved using reversed-phase column (NOVA-PAK $C_{18}$, Waters Co.) and AcCN : H$_{2}$O : AcOH (53.0:46.5:0.5) as a mobile phase. The mixture of these derivatives were separated within 35 minutes and the optimum wavelength($\lambda_{max}$ ) of the UV detector was 353 nm. The linearity of response for derivatives of Nebramycin factors is demonstrated for concentrations up to 500 $\mu\textrm{g}$/ml and the relative standard deviation is less than 0.79%. Detection limit was 1.67 ng for the 10 $\mu\textrm{l}$ sample volume employed.

• Analytical Science and Technology
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• v.18 no.6
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• pp.453-459
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• 2005

Phenol compounds in water were simultaneously analyzed by extractive derivatization. Aqueous solution was controlled to pH 13 with sodium hydroxide, and then $500{\mu}L$ of benzoyl chloride was added to the solution. The solution was shaken for 15 minutes and extracted with diethyl ether and then analyzed using GC/MS-SIM. The calibration curves of phenolic compounds in the range of 0.05 to $5.0{\mu}g/mL$ showed a good linearity having the correlation coefficient of $r^2=0.9915$ and standard deviation of ${\leq}8.5%$, respectively. The recoveries by this method ware 58.4-114.0%.

• Analytical Science and Technology
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• v.26 no.4
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• pp.228-234
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• 2013

Methamphetamine is an amine-containing illegal drug and is distributed unlawfully in South Korea. Finding a rapid, convenient and semi-quantitative determination method for methamphetamine is a very important issue in the area of forensic drug testing. As an effort to develop new screening method, the reactions between three organic compounds which are structurally similar to methamphetamine and N-(9-fluorenylmethoxycarbonyloxy) succinimide (FMOC-NHS) were performed on silica gel ($SiO_2$) TLC plates. Three reference compounds were synthesized and used for the identification, comparison and study of the limit of detection (LOD) of the products obtained from a direct reaction on a TLC plate. As a result, FMOC-NHS as a derivatization reagent generated compounds containing highly UV-active functional groups on the TLC plate after reacting with primary- and secondary amines. In the experiment 2D the LOD of amines was in the range of 0.045 and 0.01 mg/mL ($2{\mu}L/spot$), and in 1D the LOD was in the range of 0.002 and 0.007 mg/mL ($2{\mu}L/spot$). The LODs of the compounds tested were dependent on the concentration of the derivatizing reagent.