• 대한약학회:학술대회논문집
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• 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.1
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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)

• 분석과학
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• 제26권1호
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• pp.80-85
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• 2013

본 연구는 유해화학물질관리법에 지정되어 있는 사고대비물질에 대한 실험실적 분석방법을 정립하기 위한 것으로, GC/MS 분석이 가능한 25종 사고대비물질을 대상으로 정량분석을 수행하였다. GC/MS 정량분석결과 69종 사고대비물질 중 산화프로필렌(propylene oxide) 등 21개 물질에 대한 결정계수($r^2$)는 0.998 이상을 보였고, 포스겐(phosgene)의 결정계수는 0.994, 노말-부틸아민(n-butyl amine) 외 1종은 0.987, 에틸렌디아민(ethylene diamine)은 0.958의 결정계수를 보였다. 동일한 GC/MS 분석 조건으로 표준물질을 분석한 결과 총 25종에 대한 검량선이 작성되었다. 현재 사고대비물질에 대한 분석 연구가 필요한 상황에서, 본 연구결과는 화학사고 사후 환경 영향 조사를 위한 정량분석에 도움이 될 것으로 판단된다.

• 한국환경보건학회지
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• 제35권4호
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• pp.322-333
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• 2009

In this study, a measurement method was evaluated for the determination of polycyclic aromatic hydrocarbons (PAHs) in the ambient atmosphere. PAHs were sampled by high-volume samplers, and were then analysed with a GC/MS system. Particulate PAHs were collected on $8"{\times}10"$ quartz fiber filter, while vapor phase PAHs were adsorbed on polyurethane foam (PUF). Target compounds included a total of 36 PAHs, which are known to be frequently detected in the urban atmosphere. It was not necessary to clean-up samples before samples were analyzed using GC/MS, and the overall performance of the method was tested by a variety of quality control and quality assurance schemes. It is generally known that the clean-up procedure can negatively affect the recovery of samples. Precision and accuracy was evaluated using SRM provided by US NIST, and the results were generally satisfactory and reliable. However, the GC/MS method appeared not to be adequate for 6-rings PAHs, such as coronene, due to its lower sensitivity. In addition, collection efficiencies for low molecular compounds, such as 2-rings PAHs, were poor because of the lower retention volume of the PUF adsorbent. As a result, it was concluded that the method based on high-volume sampling and GC/MS analysis can give very reliable data by simultaneous sampling of both particulate and vapor phases for 3-rings to 5-rings PAHs of environmental concern.

• 한국환경농학회지
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• 제39권2호
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• pp.142-169
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• 2020

BACKGROUND: A new analytical method has been developed to determine 261 pesticide residues in herbal medicines. METHODS AND RESULTS: The extraction of pesticides was carried out by modified method of the Korea Food Standards Codex sample extraction and determination was performed using GC-MS/MS and LC-MS/MS. During the pre-treatment process of the test method, Solid-liquid separation was changed to centrifugation. The method was validated by the precision and accuracy results. 261 pesticides spiked at three level 20, 50, 100 ug/kg in herbal medicines. The limit of quantification of method were 4-40 ug/kg for GC-MS/MS and 2-45 ug/kg for LC-MS/MS, respectively. Among the pesticides analysed by GC-MS/MS and LC-MS/MS, 244 pesticides (94% of total number) in chinese matrimony vine and 224 pesticides (86% of total number) in korean angelica root and 231 pesticides (89% of total number) in jujube and 214 (82% of total number) in cnidium showed recoveries in the range of 70-120% with RSD⪯20%. CONCLUSION: These results indicated that GC-MS/MS and LC-MS/MS analysis with the sample extraction in this study can be applied to multi-residue analysis of pesticides in herbal medicines.

• 분석과학
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• 제21권5호
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• pp.403-411
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• 2008

방사성 액체폐기물의 용매추출 공정에서 발생되는 방사선 분해현상을 연구하기 위하여 추출제로 사용되는 dimethyldibutyltetradecylmalonamide (DMDBTDMA)를 합성하고, 합성된 DMDBTDMA를 $^{60}Co$ 감마 방사선으로 조사시킬 때 생성되는 방사선 분해산물을 정량 분석하였다. 방사선 조사된 DMDBTDMA에 대한 FT-IR 스펙트럼과 EI-질량스텍트럼 및 GC/MS-SIM 방법으로 측정한 결과를 바탕으로 n-methylbutylamine, tetradecane, 1-tetradecanol 3종의 방사선 분해산물의 존재를 확인하였다. 3종의 방사선 분해산물 농도는 이들 표준물질과 n-dodecane을 내부표준물질(ISTD)로 사용하여 GC/MS-SIM 방법으로 정량 분석하였다. 방사선 분해산물에 대한 총 이온 크로마토그램에서 나타난 머무름 거동, 분리도와 해상도 측면에서 만족스런 결과를 얻었으며, 총 이온 크로마토그램에서 n-methylbutylamine, n-dodecane, tetradecane 및 1-tetradecanol 각각의 성분에 대한 피크 검출시간은 각각 2.35분, 8.83분, 10.68분 및 12.75분 이었다. 그리고 tetradecane은 방사선 분해산물의 농도가 DMDBTDMA의 방사선 흡수선량과 비례하는 상관관계를 확인하였다.

• 대한화학회지
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• 제44권1호
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• pp.24-29
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• 2000

요쿠르트는 항암 및 다양한 건강 증진효과를 나타내는 것으로 알려져 있다. 요쿠르트 유산균에 의하여 생성되는 다당류(polysaccharides)가 그러한 효과를 나타내는 것으로 믿어진다. 본 연구에서는 시중에 판매되는 요쿠르트 제품중 주요한 몇 가지를 선택하여 그 속에서 다당류를 추출하고 완전산분해하여 단당류 조성비를 결정하였다. 요쿠르트 제품을 원심분리 후, 거르고 1M 황산으로 완전 산가수분해한 후 중화시켜 당용액을 얻어내었다. 이 당용액으로부터 일정량을 분취하여 증발건조시킨 후 TMSl(trimethylsilylimidazole)로 유도체화시켜 GC/MS로 분석하였다. 이번 연구에서 요쿠르트의 단당류는 fructose와 glucose 그리고 galactose로 구성되었음을 확인하였으며, 요쿠르트 제품에 따라 각기 다른 단당류 조성비 결과를 주었다.

• 한국수정란이식학회지
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• 제29권2호
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• pp.195-200
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• 2014

Endothelin 2 (EDN2) induces follicular rupture by constricting periovulatory follicles. In this study, it was investigated the mechanisms of EDN2 action on follicular rupture with respect of receptor using the conditionally granulosa cell specific EDN2 receptor type A (ETa) KO mice (gcETaKO; $ETa^{flox/-}{\cdot}Amhr2^{Cre}$). It was generated the gcETaKO mice by breeding with $ETa^{flox/-}$ mice after mono-alleic ETa knockout by $ZP3^{Cre}$ and $Amhr2^{Cre}$ mice. Fertility, ovulation and maturation rates of ovulated oocytes after super ovulation were investigated in the gcETaKO mice compared with wild-type mice ($ETa^{flox/flox}$ and $ETa^{flox/-}$) as a control group. In the gcETaKO mice, normal fertility after breeding with male mice was shown compared with wild-type mice. And, there was no significant differences in ovulation rates after super ovulation, however its maturation rates was lower than that of wild type mice. These findings show that EDN2 in follicular rupture for ovulation is related with an other ETa not in granulosa cells. Further studies are needed to investigate how EDN2 is acted in ovarian follicular rupture for ovulation.

• Bulletin of the Korean Chemical Society
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• 제23권3호
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• pp.488-496
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• 2002

SPME techniques have proven to be very useful tools in the analysis of wide VOCs in the air. In this study, we estimated VOCs in ambient and workplace air using a Tedlar ba /SPME/GC/MS system. The calibration curve was set to be linear over the range of 1-30 ppbv. The detection limits ranged from 10 pptv to 0.93 ppbv for all VOCs. Reproducibility of TO-14 target gas mixtures by SPME/GC/MS averaged at 8.8 R.S.D (%). Air toxic VOCs (hazardous air pollutants, HAPs) containing a total of forty halohydrocarbons, aromatics, and haloaro-matic carbons could be analyzed with significant accuracy, detection limit and linearity at low ppbv level. Only reactive VOCs with low molecular weight, such as chloromethane, vinylchloride, ethylchloride and 1,2-dichloro-ethane, yielded relatively poor results using this technique. In ambient air samples, ten VOCs were identified and quantified after external calibration. VOC concentration in ambient and workplace air ranged from 0.04 to 1.85 ppbv. The overall process was successfully applied to identify and quantify VOCs in ambient/workplace air.

• 한국동물위생학회지
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• 제28권3호
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• pp.285-294
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• 2005

This study was conducted to investigate the extraction method for the determination of organochlorine, organophosphorus and synthetic pyrethroid pesticide residues in beef fat by gas chromatography-mass selective detector(GC-MSD). Twenty one pesticide residues in fat were determined using a simple and rapid procedure based on solid- phase extraction(SPE) clean-up cartridges with octadecyl $(C_{18})-bonded$ porous silica, florisil, $10\%$ deactivated florisil. a tandem $C_{18}$ and florisil and a tandem $C_{18}$ and $10\%$ deactivated florisil. Solvent-solvent extraction using acetonitrile was not satisfied to eliminate fat interference for pesticide residue analysis by GC-MSD, and the recoveries of the method in fat ranged from 16.2 to $57.3\%$ except DDT$(83.2\%)$. The recoveries of SPE methods using a tandem $C_{18}$ and Florisil was $59.6\~123.8\%$ except fenitrothion $(135.2\%)$. the SPE method was verified the satisfactory performance of pre-treatment for pesticide residues analysis in fat by GC-MSD. The efficiency of florisil deactivated with $10\%$ water has been not proved significantly on recoveries of pesticide residues in fat.

• 약학회지
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• 제47권3호
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• pp.142-147
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• 2003

Gas chromatography-mass spectrometric (GC-MS) procedure is presented for the simultaneous qualification and quantitation of methamphetamine (MA), amphetamine (AMP), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA), and 3,4-methylenedioxyethylamphetamine (MDEA) in human hair. The method procedure involves decontamination of hair with distilled water and acetone, acidic hydrolysis, extraction in the presence of deuterated internal standards, and GC-MS analysis after derivatization with trifluoroacetic anhydride (TFAA) in ethylacetate. The limit of detection for 5 drugs were about 0.1∼0.15 ng/mg using 30 mg hair sample. Coefficient variations of correlation ranged from 0.9941 to 0.9993. The recoveries of these drugs were found to be 93.4∼104.4％. The concentrations of AMP, MA, MDA, and MDMA in abusers' hair samples were measured 0.17∼2.88, 2.09∼18.34, 0.24∼3.83, and 3.10∼22.81 ng/mg, respectively. The ratios of MA/AMP and MDMA/MDA ranged 5.67∼49.57 and 4.78∼54.31, respectively. This assay has been successfully utilized in the evaluation of the deposition of amphetamine-type stimulants (ATS) in human hair.