• 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.

• Journal of the Korean Society of Clothing and Textiles
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• v.31 no.6 s.165
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• pp.859-868
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• 2007

Degradation products of the dye extracted from turmeric and the turmeric dyed textiles were examined by using GC-MS after 100 oven (OV) and $H_2O_2/UV/O_2$(PER) treatments for up to 28 days. Throughout the OV degradation times, 2-propenoic acid, 3-(2-hydroxyphenyl)- was found consistently, while isovanillin, and vanillic acid were newly detected. In 28 day PER degradation sample, feruloylmethane, 2-propenoic acid, 3-(2-hydroxyphenyl)-, benzoic acid, and vanillic acid were detected as well as isovanillin. Feruloylrnethane, and 2-propenoic acid, 3-(2-hydroxyphenyl)- were detected from the degraded fabric samples. With the absence of curcuminoids in the GC-MS result, the decreasing pattern of 2-propenoic acid, 3-(2-hydrokyphenyl)- reflect the degradation of curcuminoids in turmeric extraction with the progression of OV degradation times. It is suggested that isovanillin, feruloylmethane, 2-propenoic acid,3-(2-hydroxyphenyl)-, and vanillic acid are the probable fingerprint products for determining the turmeric dye from the badly faded archaeological textiles.

• Analytical Science and Technology
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• v.13 no.1
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• pp.108-120
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• 2000

To perform an effective screening for toxic materials of forensic interest detected in high profile criminal case in biological and environmental samples, we tried to construct a searchable computerized database using HPTLC(High Performance Thin Layer Chromatography) and GC/MS. Retardation factor($R_f$) values and UV spectral data of HPTLC were investigated for 160 pesticides, 34 chemicals and 39 explosives of standard grade. The data were compiled in a library. We also analyzed 112 pesticides, 31 chemicals and 17 explosives and 57 volatile organic compounds(VOCs) by GC/MS. The data for RT and characteristic mass ions were also compiled in a library.

• Journal of Life Science
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• v.17 no.5 s.85
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• pp.619-624
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• 2007

Species of genus Acanthopanax(Araliaceae) are long-lived trees primarily distributed throughout East Asia. These species are regarded as medically and ecologically important in Korea. A variety of Cheongsong in Korea is one of these cultivated varieties, however this variety is much longer(>100 years) than those of other cultivated groups. The components of variety of Acanthopanax in Cheongsong were analyzed for the first time and were compared to those of all Acanthopanax taxa in Korea. Nineteen components were specific to variety in Cheongsong. The main components of this variety were $\beta$-caryophyllene, hexadecanoic acid and ethyl stearate. Although some components are differ from each other, variety Cheongsong was similar to A. senticosus at phonetic topology with content of the chemicals, In addition, six species of genus Acanthopanax were investigated to compare the major chemical components by GC-MS.

• Analytical Science and Technology
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• v.34 no.2
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• pp.68-77
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• 2021

Cannabis is one of the most abused drugs in Korea. The main psychoactive component in cannabis, Δ9-tetrahydrocannabinol, is metabolized to 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THCCOOH) and THCCOOH-glucuronide (THCCOOH-glu) in the human liver, whereby the amount of THCCOOH-glu found in urine is twice as high as that of THCCOOH. The analytical process adapted by the majority of urine drug-testing programs involves a two-step method consisting of an initial immunoassay-based screening test followed by a confirmatory test if the screening test result is positive. In this study, a qualitative gas chromatography-mass spectrometry (GC-MS) method was developed and validated for the detection of THCCOOH in human urine, where THCCOOH-glu was converted into THCCOOH by alkaline hydrolysis. For purification of the urine extract prior to instrumental analysis, high-speed centrifugation was used to minimize interference. In addition, an injection-port derivatization method using ethyl acetate and N,O-bis(trimethylsilyl)-trifluoroacetamide containing 1 % trimethylchlorosilane was employed to reduce the time required for derivatization, and an aliquot of the final solution was injected into the GC-MS. The method was validated by measuring the selectivity, limit of detection (LOD), and repeatability. The sensitivity, specificity, precision, accuracy, Kappa, F-measure, false positive, and false negative rate were determined by comparing the GC-MS results with those obtained using the immunoassay. The LOD was determined to be 0.32 ng/mL, while the repeatability was within 9.1 % for THCCOOH. Furthermore, a comparison study was carried out, whereby the screening immunoassay exhibited a sensitivity of 86.4 % and a specificity of 100 % compared to GC-MS. The applicability of the developed method was examined by analyzing spiked urine and forensic urine samples obtained from suspected cannabis abusers (n = 221).

• Analytical Science and Technology
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• v.24 no.3
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• pp.183-192
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• 2011

This study was done for the determination and excretion profile of superdrol and its metabolites in human urine using both liquid chromatography with electrospray ionization mass spectrometry and gas chromatography with mass spectrometry after trimethylsilylation. Superdrol and its two metabolites were detected in human urine after administration of superdrol to healthy volunteers. The intra-day recovery ranged 89.7-113.2%, accuracy ranged 91.8-113.8% and reproducibility ranged 0.2-6.8% and inter-day recovery ranged 89.3-104.1%, accuracy ranged 95.2-103.0%, reproducibility ranged 0.7-7.8%. We found that superdrol M1 was a hydration at C-3 and superdrol M2 was a hydroxylation at D-ring. Superdrol and two metabolites were excreted as their glucuronided fractions. The glucuro-/sulfa-conjugated ratio of superdrol, superdrol M1 and superdrol M2 were 0.02, 0.02, 0.01, respectively. The excretion studies showed that superdrol and two metabolites were reached 4.3 h after oral administration and superdrol and superdrol M1 were detected until 48 h in human urine.

• Korean Journal of Pharmacognosy
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• v.38 no.4
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• pp.327-333
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• 2007

The chemical composition of the volatile constituents from the leaves, stems, and roots of Acanthopanax senticosus growing wild in Mt. Deok-Yu was determined by GC and GC/MS spectrometric analysis with the aid of NBS, Wiley Library and RI indice searches. The major constituents identified were ${\delta}-elemene\;(23.14%),\;{\beta}-elemene\;(5.59%),\;{\gamma}-cadinene\;(5.43%),\;and\;{\alpha}-bergamotene\;(28.54%)$ in the leaves, ${\alpha}-pinene\;(11.50%),\;{\delta}-elemene\;(17.62%),\;{\alpha}-bergamotene\;(27.21%)$, and bicycloheptane derivative (6.38%) in the stems, and ${\alpha}-pinene\;(21.90%)$, and (+)-aromadendrene (3.77%) in the roots.

• Food Quality and Culture
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• v.1 no.1
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• pp.13-17
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• 2007

The volatile flavor compounds of Saussurea lappa C.B. Clarke, a perennial, aromatic and medicinal herbaceous plant of the Asteraceae family, were isolated by the hydro distillation extraction method using a Clevenger-type apparatus, and analyzed by gas chromatography (GC) and gas chromatography-mass spectrometry (GC/MS). The plant yielded a light yellow colored oil (0.02%, v/w). From S. lappa C.B. Clarke root oil, sixty-three volatile flavor compounds were tentatively identified, among which sesquiterpene was predominant (21.70%). The identified compounds of the root oil constituted 87.47% of the total peak area. From the constituents making up more than 5% of the volatile flavor components, a long-chain aldehyde, (7Z, 10Z, 13Z)-7, 10, 13-hexadecatrienal, was the most abundant volatile flavor compound (21.20%), followed by dehydrocostuslactone (10.30%) belonging to sesquiterpene lactone, valerenol (5.30%) and vulgarol B (5.06%).

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.11 no.3
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• pp.206-211
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• 2001

This article describes identification and quantification of benzene in the casting process. Air samples around the casting process were taken by using personal air sampler attached charcoal tube and desorbed by carbon disulfide. The identification and quantitative analysis of benzene have been performed by GC-MS and GC-FID. Calibration range of standard solutions for benzene was prepared in range from 0.1 to 2 times of TLVs concentrations($1.4{\sim}28{\mu}g/1m{\ell}$ CS2) and the limit of detection was $0.11{\pm}0.002{\mu}g/1m{\ell}$ CS2. Benzene detected in airborne was ranged in 4.0ppb~104.7ppb.

• Analytical Science and Technology
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• v.25 no.5
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• pp.292-299
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• 2012

GC/MS has been utilized for many applications due to great resolution and reproducibility, which made it possible to build up the database of mass spectrum, while HS-SPME has the advantage of solventfree extraction of volatile compounds. The combination of these two methods, HS-SPME GC/MS, enabled many scientific applications with various possibilities. In this study, the analysis of trail pheromone excreted from live Camponotus japonicus with the feature of solvent-free extraction was carried out and the optimization for this analysis was performed. The major compounds detected were n-decane, n-undecane, and n-tridecane. Optimization for the best detection of these hydrocarbons was processed in the point of SPME parameter (selection of fiber, extraction temperature, extraction time, etc.). The advantage of the analysis of live sample is to analyze phenomenon right after it is excreted by ants. But the experimental process has restriction of extraction temperature and time because of the analysis of live ants. Establishing the process of HS-SPME GC/MS applied to live samples shown in this study can be a breakthrough for the ecofriendly and ethical research of live things.