• Korean Journal of Plant Resources
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• v.8 no.2
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• pp.115-125
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• 1995

The moistures, colors and flavors of red pepper were analyzed to observe the changes of the qualities of red pepper with various conditions of drying. The moisture was 11.8%, known as optimal condition for storing red pepper, where dried at $50^{\circ}C$ for 36 and 48 hours. The color of red pepper air-dried at 50% for 48 hours was estimated to be the most execllent in comparison of sun drying and air drying. The optimal absorbances of hexnae extract from red pepper were examined. The ratios between the absorbances at 280nm and at the typical wavelengths of caretenoids(430nm, 450nm, 474nm) were from 2.5-3.4 and these wete also confirmed by the sight of the eye. Hexane fraction showed more peaks of flavors than benzene fraction and both of the two were silylated by with BSTFA to analyze the flavors by GC. CG profiles for the compositions of flavors in red perpper are thought to be useful for extimating the quality of favors in red pepper. Eight flavors including benzene dicarbozylic acid, were identified from red pepper and major components of them were oleic palmitic acids. Drying temperatures and times did not have effects on the changes of specific flavor components but did influenced the compositions of them in red pepper.

• Analytical Science and Technology
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• v.23 no.6
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• pp.544-550
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• 2010

Mistaking pink colored thermal oil for grape wine, a victim drank the oil to death which was analyzed to contain 39% of ethylene glycol. Thermal oil could be used for heat transfer to prevent the malfunction due to the high pressure in the boiler operated at high temperature when using water. Main component of thermal oil is known to be mineral oil or ethylene glycol. From the blood and other tissue of the victim from autopsy, ethylene glycol and its metabolite were simultaneously analyzed by GC/MS after extraction under acidic condition with acetonitrile followed by derivatization with BSTFA. About 0.2 g of the specimens were pretreated with 50 uL of 0.5 M HCl solution to keep acidic condition, then dehydrated with anhydrous sodium sulfate followed by concentration under nitrogen stream. Ethylene glycol and glycolic acid concentration in blood was measured to be $2,755\;{\mu}g/mL$ and $174\;{\mu}g/mL$ respectively. In other specimen, the concentration of ethylene glycol and glycolic acid was $860\;{\mu}g/g\sim1,290\;{\mu}g/g$ and $93\;{\mu}g/g\sim134\;{\mu}g/g$. Especially, crystal appeared in kidney which was supposed xalate from the metabolite of ethylene glycol.

• Analytical Science and Technology
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• v.22 no.3
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• pp.219-227
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• 2009

The steroid compounds in Rhodiola sachalinensis were determined with adsorption column chromatographic purification and GC/MS. Sterols were extracted by sonication and Soxhlet with ethanol and dichloromethane, respectively. The extract was partitioned with chloroform and water using liquid-liquid extraction, and purified with a silica column after the sterols had been converted to the corresponding silyl derivatives with BSTFA. Eighteen free sterols, including $\beta$-sitosterol, stigmasterol and cycloartenol, and nine sterol conjugates were found from Rhodiola sachalinensis by GC/MS. Among them, cholest-5-ene-3-ol, cholesterol, stigmasterol, $\beta$-sitosterol were confirmed and quantified with sterol standards. Most sterols were presented in the chloroform part, with $C_{29}$ being the most abundant group in this sterol group. $\beta$-sitosterol was the most abundant compound with a relative content of 45.94% followed by ergost-7-ene-3-ol (11.33%), 4,14-dimethyl-ergosta-8,24(28)-diene-3-ol (7.07%), stigmasterol (6.09%), cycloartenol (5.43%) and 4-methyl-cholest-5-ene-3-ol (5.39%).

• Journal of The Korean Society of Inherited Metabolic disease
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• v.15 no.3
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• pp.138-146
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• 2015

Purpose: If early diagnosis is not made, patients with metabolic disorders as homocystinemia rapidly progress to physical defect or mental retardation resulted in storage of the toxic material into the brain. Therefore, it is necessary to develop an analytical method for a rapid screening and/or correct confirmation diagnosis. Methods: The standard solution of sulfur amino acids spiked plasma was subjected to protein precipitation with methanol, and then consecutively derivatized with trimethylsilyl (TMS) and trifluoroacyl (TFA) and determined by GC-MS. The formation of TMS derivative of the hydroxyl and TFA derivative of amino functional group was performed by BSTFA and MBTFA, respectively. Selective ion monitoring (SIM) mode was used for quantification with selected specific ions. Results: A calibration curve on standard spiked pooled plasma showed a linear relationship with correlation coefficient of 0.9936-0.9992 for all compounds over the range of 0.1-300 ng. The precision and accuracy were within S.D. of 1-15% and RSD of 1-15% for intra-day assay at 2 ng/mL, 15 ng/mL and 30 ng/mL. LOD and LOQ was 0.4 ng/mL and 4 ng/mL respectively. Conclusion: A rapid analytical method was developed to quantify sulfur amino acids and methyl malonic acid, after two-step derivatization procedure with good sensitivity and specificity on human plasma. Advantages of a new method are simplicity and rapidity. The method could be useful for routine analysis, diagnosis of homocysteinemia.

• Applied Biological Chemistry
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• v.35 no.2
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• pp.132-138
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• 1992

For effective determination of methylthiohydantoin amino acids(MTHs) by gas liquid chromatography in the protein sequencing, derivatization with N-methyl-N-(tert.-butyl-dimethylsilyl)trifluoroacetamide(MTBSTFA), a new silylating reagents, was attempted instead of trimethylsilyl(TMSi) derivatives by N,O-bis(trimethylsilyl)trifluoroacetamide(BSTFA) used up to the present and N(O)-butyldimethylsilyl MTHs derivatized by MTBSTFA were analysed on HP-1 capillary column. Twenty one protein amino acids except cystine were indentified. Especially arginine that did not detected with TMSi derivative on packed column until now was resolved by derivatization with MTBSTFA. N(O)-butyldimethylsilyl MTHs showed multiple peaks by MTBSTFA were proline, isoleucine, glycine and tyrosine and hydroxyproline especially showed several extraneous peaks more than two. Calibration curves of N(O)-butyldimethysilyl MTHs of amino acids in the range of $2.5\;nmol{\sim}7.5\;nmole$ showed good linearity. however, those of lysine, histidine and arginine showed linearity in the range of $5.0\;nmole{\sim}15.0\;nmole$. Correlation coefficients and regression coefficients of all calibration curves were highly significant(p<0.001).

• YAKHAK HOEJI
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• v.52 no.3
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• pp.172-175
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• 2008

Stable isotope ratio of carbon and nitrogen ($\delta^{13}C$ & $\delta^{15}N$), and $\Delta^{9}$-tetrahydrocannabinol (THC) contents were measured on 37 Korean cannabis and 10 commercial grade marijuana seized in Korea. Factors influencing on the measured values and their variations were investigated. $\delta^{13}C$ value of cannabis is specified mainly by water availability. Korean cannabis showed relatively low $\delta^{13}C$ values ranging -33.29$\sim$-27.01% (mean=-31.01%), which reflect geographic conditions of Korea where is rainy, especially during summer. $\delta^{15}N$ values, which reflect individual planting conditions, were relatively high up to -0.5$\sim$18.0% (mean=6.44%). It reflects characteristics of Korean cannabis growing wild in forest or cultivated in fertile soil. Tetrahydrocannabinol is the major hallucinogenic compound of cannabis. Ethanol extracts of cannabis leaves were derivatized by N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA), and the derivatives were analyzed by GC-MS in selected ion monitoring (SIM) mode. THC contents of Korean cannabis ranged 0.11$\sim$4.34% (mean=1.47%), which were relatively low compared with commercial grade marijuana.

• YAKHAK HOEJI
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• v.48 no.3
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• pp.207-212
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• 2004

An analytic method was developed for the quantitation of $\Delta$$^{9}-$ tetrahydrocannabinol (THC) and 11-nor-9-carboxy THC (THC-COOH) in human hair. After hair samples were pulverized using Freezer Mill, deuterated internal standards were added and digested in 1 N NaOH at $100^{\circ}C$ water bath for 30 min. Digest solutions were extracted by 5 ml hexane：ethyl acetate (90：10) after acidification with acetic acid. The organic phase was evaporated under N 2 and derivatized by BSTFA (with 1% TMCS) at $85^{\circ}C$ for 45 min. The derivatized solution was separated on HP-5MS column ($30m{\times}0.25mm{\times}0.25mm$) and detected using EI-GC-MS with selective ion monitoring mode. The assay of calibration was ranged from 5 to 100 ng/50 mg hair ($r^2$＞0.99) for THC and THC-COOH. Within and between-run precision were calculated at 6, 30, 60 ng/50 mg hair with coefficients of variation less than 11%. Within and between run accuracies at the same concentrations were$\pm$14% and $\pm$30% of target for both analytes, respectively. Absolute and relative recovery at 10 and 100 ng were 60∼91％. The method was used to detect and quantify THC and THC-COOH in cannabis abuser's hairs (N = 16) and SRM (N=5, THC 1 ng/mg, NIST). We detected THC and THC-COOH in only one hair sample. In SRM, % accuracy was 93% (range 86∼103%) and precision (% CV) was 8.14. We began to set up a quantitative analysis of THC and THC-COOH using EI-GC-MS. Continuously, we need to modify and develop this method in order to apply for identification in cannanbis users' hair.

• Analytical Science and Technology
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• v.28 no.5
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• pp.323-330
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• 2015

Alkaptonuria, a rare inherited metabolic disease, is characterized by a lack of homogentisate dioxygenase and accumulation of homogentisic acid (HGA), leading to homogentisic aciduria, arthritis, and ochronosis. In this study, a rapid analytical method, without an expensive and tedious solid phase extraction step, was developed to quantify HGA in plasma using GC-MS. HGA-spiked pooled plasma samples were subjected to liquid-liquid extraction (LLE) with ethyl acetate, followed by trimethylsilyl derivatization (TMS) and GC-MS quantification using selected ion monitoring. The formation of TMS derivative of the 1 carboxylic and 2 hydroxyl functional groups was performed by reacting BSTFA (with 10% TMCS) for 5 min at 80 ℃. For selected ion monitoring, quantification and confirmation ions were determined based on specific ions (m/z 384, m/z 341 and m/z 252) of the TMS derivative of HGA. Calibration curves of pooled normal plasma specimens showed a linear relationship in the range of 1-100 ng/µL. The precision and accuracy were within a relative standard deviation (RSD) of 1 to 15% and a bias of -5 to 25%. Recoveries were obtained in the range of 99-125% and 95-115% for intra-day and inter-day assay, respectively, at 2, 20 and 80 ng/µL. The limit of detection (LOD) and limit of quantification (LOQ) were 0.4 ng/µL and 4 ng/µL, respectively. No homogentisic acid was excreted from normal Korean plasma samples. Collectively, the results from the present study suggest that this method could be useful for routine diagnosis and therapeutic monitoring of alkaptonuria patients with excellent sensitivity and rapidity.

• Analytical Science and Technology
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• v.23 no.2
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• pp.179-186
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• 2010

The oxidative metabolism of ibuprofen in healthy male urine collected at 3, 6, 9, 12 and 15 h after oral administration of ibuprofen was studied by GC/MS assay. To detect conjugated metabolites of ibuprofen, urine sample was acid-hydrolyzed with 6 M HCl at $100^{\circ}C$ for 30 min. To effectively extract ibuprofen and its metabolites, liquid-liquid extraction (LLE) was conducted at pH 3, 5, and 7, respectively. As a result, LLE at pH 3 was shown to be the best extraction condition. For the determination of trace amounts of ibuprofen and its metabolites in extract, trimethylsilylation (TMS) with BSTFA was applied and followed by GC/MS analysis. In this study, main 5 metabolites including parent drug were detected and these metabolites were assigned as three hydroxylated forms and one carboxylated form. Each metabolite was tentatively identified by both interpretation of mass spectrum and comparison with previously reported results. In addition, time profile of urinary excretion rate for parent drugs and metabolites was studied. Finally, the metabolic pathways of ibuprofen were suggested on the basis of the structural elucidation of its metabolites and excretion profiles.