• Analytical Science and Technology
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• v.19 no.1
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• pp.107-114
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• 2006

Early diagnosis and medical intervention are critical for the treatment of patients with metabolic disorders. A rapid analytical method was developed for simultaneous quantification of organic acids and amino acids in urine without labor-intensive pre-extraction procedure showing high sensitivity and specificity. A new method consisted of simple two-step trimethylsilyl (TMS)-trifluoroacetyl (TFA) derivatization using GC/MS-selective ion monitoring (SIM). Filter paper urine specimens were dried under nitrogen after being fortified with internal standard (tropate) in a mixture of distilled water and methanol. Methyl orange was added to the residue as indicator reagent. Silyl derivative of carboxylic functional group was followed by trifluoroacetyl derivative for amino functional group. N-methyl-N-(trimethylsilyl-trifluoroacetamide) and N-methyl-bistrifluoroacetamide were consecutively added and heated for 15-20 min at $65^{\circ}C-70^{\circ}C$, for TMS-TFA derivative, respectively. This reactant was analyzed by GC/MS-SIM. Linear dynamic range showed 0.001-50 mg with the detection limit of (S/N=3) 10-200 ng, and the quantification limit of 80-900 ng in urine. Correlation coefficient of regression line was 0.994-0.998. When the method was applied to the patients 'urine, it clearly differentiated the normal from the patient with metabolic disorder. The study showed that the developed method could be the method of choices in rapid and sensitive screening for organic aciduria and amino acidopathy.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.22 no.2
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• pp.153-160
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• 1996

A novel simple method to detect vitamins in cosmetic products by gas chromatography-mass spectrometry(GC-MS) has been developed. Three vitamins(panthenol, cholecalciferol and tocopherol) were used for this study. Vitamins were prepared by dissolving in tetrahydrofuran(THF), and silylated with bis-trimethylsilyltrifluoroacetamide-trichloromethylsilane(BSTFA). Silated vitamins were separated on a fuses-silica capillary column coated with DB-5. The identification of each vitamin was accomplished by retention time and mass spectrum library search with a computer, and the quantitation was made in the selected-ion monitoring(SIM) mode of GC-MS. SIM mode had given sensitivity to determine 50pg of panthenol, 285pg of cholecalciferol and 130pg of tocopherol. Linearity was maintained over the range 0.005-0.20% for each vitamin. Each cosmetic product(i.e. hair tonic and lotion) was found to contain amounts of the vitamins. This method was sensitive and gave 77.5-99.9% recovery of each vitamin from these cosmetic products. From these results, we concluded that silylation with BSTFA followed by GC-MS analysis allows the simple, covenient and exact determination of panthenol, cholecalciferol and tocopherol.

• Proceedings of the PSK Conference
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• 2003.04a
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• pp.169.2-169.2
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• 2003

A method using EI-GC-MS is described for the determination of amphetamines in hair. The method is applied to simultaneous quantify amphetamines (methamphetamine, amphetamine, MDMA and MDA). Drugs were extracted in 1 ％ HCl in methanol from hair. After derivertization with TFAA, the resulting drugs were separated on HP-5MS column during a 16 min program and identified by mass spectrometry with the SIM mode(EI-GC-MS). (omitted)

• Journal of the Korean Society of Clothing and Textiles
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• v.33 no.6
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• pp.980-989
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• 2009

Amur cork tree was extracted in methanol with the purpose of investigating the most effective extraction procedure for detecting the chromophore using the GC-MS analysis. Different procedures of waterbath and hotplate extractions were carried out and five different GC-MS instrument parameters including the operating temperatures in the GC capillary column and the MSD scan range were tested for their efficiencies. Berberine was determined by the detection of dihydroberberine at 15.0 min r.t. Hotplate was a better device for extracting amur cork tree than waterbath shaker either with or without presoaking in the room temperature. Water was not an adequate extraction medium for the berberine detection. The most effective GC-MS parameter was Method 4; the initial temperature at $50^{\circ}C$ followed by the temperature increase of $23^{\circ}C$/min until $210^{\circ}C$, then increase of $30^{\circ}C$/min until the final temperature reach at $305^{\circ}C$, then hold for 14 minutes to maintain the total run time 24.12 minutes. The MSD scan range for Method 4 was $35\sim400$m/z.

• Journal of Environmental Health Sciences
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• v.28 no.1
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• pp.21-29
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• 2002

To identify and evaluate the dichlorobenzidine(DCB)-DNA adducts in liver cell and bladder epithelial cells by $^{32}$ P-postlabeling and GC/MS-SIM, we orally exposed the dichlorobenzidine(20mg/kh body wt./day) to male Sprague-Dawley rats(l85$\pm$10g) for 14 days. Two kinds of DCB-DNA adduct(A1 and A2) were found at the same site of thin layer chromatogram of $^{32}$ P-postlabeling method in liver cells and bladder epithelial cells. In liver cells, relative adduct labeling(RAL) $\times$ 10$^{12}$ of DCB-DNA adduct A1 were 34.1$\pm$3.71 and 69.9$\pm$5.02, that of adduct A2 were 74.1$\pm$10.1 and 105.1$\pm$10.1 on 10 and 14 days after treatment, respectively. And in bladder epithelia cells, RAL $\times$ 10$^{12}$ of DCB-DNA adduct A1 were 5.92$\pm$1.60 and 15.9$\pm$1.31, that of adduct A2 were 9.81$\pm$2.81 and 22.8$\pm$1.79 on 10 and 14 days after treatment, respectively. DCB metabolites formed DNA adducts were monoacetyl-dichlorobenzidine(acDCB) and diacetyl-dichlorobenzidine(di-acDCB), which was identify by gas chromatography/mass spectrometry-scan ionization mode(GC/MS-SIM), after hydrolysis of DCB-DNA adducts isolated from live cells and bladder epithelial cells. The base peak of acDCB were 252 and 294 m/z, and that of di-acDCB were 252, 294 and 336 m/z. In conclusion, the exposed DCB formed two kinds of DCB-DNA adduct, the proximate materials of that were acDCB and di-acDCB in liver and bladder epithelial cells. And the above GC/MS-SIM method was found the DCB-DNA adducts could be monitoring by gas chromatography.

• Analytical Science and Technology
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• v.24 no.4
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• pp.256-265
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• 2011

Ambers have been used as a gemstone and a religious object since the ancient times and found in several archaeological sites in Korea. To prepare an enhanced conservation measures, we surveyed the chemical and spectroscopic properties of the ambers according to the provenance. Total 14 amber samples were collected from 6 different provenances including Baltic, Chiapas, Colombian, Dominican, Fushun and Madagascar amber. Infrared (IR) spectroscopic analysis was conducted for the non-destructive examination of the amber samples. They were also analyzed with pyrolysis/GC/MS (py/GC/MS) at the pyrolysis temperature of $300^{\circ}C$ with the on-line derivatization to trimethylsilyl ester. Baltic shoulder corresponding to the absorption at $1250cm^{-1}{\sim}1150cm^{-1}$ appeared in the IR spectrum of Baltic amber. IR spectra of the other ambers also showed somewhat distinctive characteristic peaks. In py/GC/MS analysis peaks assignable to succinic acid, dehydroabietic acid and pimaric acid were detected, which are known to be the components of the amber. In the meanwhile, the presence of compounds appearing in certain amber will be applied to differentiate the provenances of amber relics if their fragments are available for the analysis. These results are expected to help the confirmation of archaeological amber relics and archaeometric interpretation of provenances and manufacturing techniques.

• Korean Journal of Food Science and Technology
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• v.28 no.2
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• pp.226-231
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• 1996

A serum-pulp method was applied to concentrate peach pulp with aroma recovery. The serum portion was concentrated to five-fold at $50{\sim}55^{\circ}C$ and $30{\sim}50$ mmHg with aroma recovery. The concentrated serum, insoluble pulp and aroma fraction were recombined to make a two-fold concentrated peach pulp. The results of GC and GC/MS analysis for volatile compounds and sensory evaluation of concentrated peach pulp indicated that flavor quality was significantly improved by addition of aroma fractions. A 10% aroma recovery appeared to be appropriate for peach pulp.

• Analytical Science and Technology
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• v.7 no.1
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• pp.65-78
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• 1994

The herbicide mixture of 7 triazines and 9 phenoxyalkanoic acid esters was simultaneously separated and determinated with the selected ion monitoring by using gas chromatography/mass spectrometry. The extraction recoveries of those herbicides from the reagent water were studied for the organic solvent extraction(LLE) with methylene chloride. The calibration curves of them showed good linearity over the concentration range of 0.2~0.5ng/ml and the detection limits were 0.2~0.5ng/ml for 100ml of water. This analytical method could be applied to the drinking water and biological sample.

• Analytical Science and Technology
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• v.33 no.1
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• pp.23-32
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• 2020

Methamphetamine (MA) is the most common and available drug of abuse in Korea and its primary metabolite is amphetamine (AP). Detection of AP derivatives, such as MA, AP, phentermine (PT), MDA, MDMA, and MDEA by the use of immunoassay screening is not reliable and accurate due to cross-reactivity and insufficient specificity/sensitivity. Therefore, the analytical process accepted by most urine drug-testing programs employs the two-step method with an initial screening test followed by a more specific confirmatory test if the specimen screens positive. In this study, a gas chromatography-mass spectrometric (GC-MS) method was developed and validated for confirmation of MA and AP in human urine. Urine sample (500 µL) was added with N-isopropylbenzylamine as internal standard and ethyl chloroformate as a derivatization reagent, and then extracted with 200 µL of ethyl acetate. Extracted samples were analysed with GC-MS in the SIM/ Scan mode, which were screened by Cobas c311 analyzer (Roche/Hitachi) to evaluate the efficiency as well as the compatibility of the GC-MS method. Qualitative method validation requirements for selectivity, limit of detection (LOD), precision, accuracy, and specificity/sensitivity were examined. These parameters were estimated on the basis of the most intense and characteristic ions in mass spectra of target compounds. Precision and accuracy were less than 5.2 % (RSD) and ±14.0 % (bias), respectively. The LODs were 3 ng/mL for MA and 1.5 ng/mL for AP. At the screening immunoassay had a sensitivity of 100% and a specificity of 95.1 % versus GC-MS for confirmatory testing. The applicability of the method was tested by the analysis of spiked urine and abusers' urine samples.

• Applied Biological Chemistry
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• v.28 no.2
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• pp.82-87
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• 1985

Aiming at the improvement of accuracy and sensitivity of gibberellin analysis by gas chromatography-selected ion monitoring (GC-SIM), the mass spectra of two types of 29 gibberellin derivatives, methyl ester-trimethylsilyl ethers and trimethylsilyl ester-trimethylsilyl ethers, were obtained and their advantages and disadvantages in GC-SIM analysis are discussed.