• Journal of Korean Society of Environmental Engineers
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• v.36 no.11
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• pp.764-770
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• 2014

This study assessed analysis of N-nitrosamines by separation, identification, and quantification using a gas chromatography (GC) mass spectrometer (MS) with electron impact (EI) mode. Samples were pretreated by a automated solid phase extraction (SPE) and a nitrogen concentration technique to detect low concentration ranges. The analysis results by EI-GC/MS (SIM) and EI-GC/MS/MS (MRM) on standard samples with no pretreatment exhibited similar results. On the other hand, the analysis of pretreated samples at low concentrations (i.e. ng/L levels) were not reliable with a EI-GC/MS due to the interferences from impurity peaks. The method detection limits of eight (8) N-nitrosamines by EI-GC/MS/MS analysis ranged from 0.76 to 2.09 ng/L, and the limits of quantification ranged from 2.41 to 6.65 ng/L. The precision and accuracy of the method were evaluated using spiked samples at concentrations of 10, 20 and 100 ng/L. The precision were 1.2~13.6%, and the accuracy were 80.4~121.8%. The $R^2$ of the calibration curves were greater than 0.999. The recovery rates for various environmental samples were evaluated with a surrogate material (NDPA-$d_{14}$) and ranged 86.2~122.3%. Thus, this method can be used to determine low (ng/L) levels of N-nitrosamines in water samples.

• Bulletin of the Korean Chemical Society
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• v.23 no.8
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• pp.1097-1102
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• 2002

The mass spectrometry using an ion trap tandem mass spectrometer has been investigated to find optimum conditions for the analysis of benzo(a)pyrene (3,4-benzpyrene). The applicability to a real soil sample was also investigated to verify the usef ulness of the MS/MS (or collision induced dissociation, CID) analysis. The optimum CID condition was 1.5 and 0.45 for the RF excitation voltage and the q value, respectively. For comparison, CID and EI were applied to the analysis of a soil sample. CID analysis was more sensitive than EI analysis of the soil sample. The limit of detection (LOD) of benzo(a)pyrene was 3.18 ng mL-1 and 0.85 ng mL,-1 for EI and MS/MS analysis, respectively. The precision at the soil sample for EI and CID showed relative standard deviations of 6.1% and 4.1%, respectively, and the concentrations were 168 ㎍ kg-1 and 162 ㎍ kg-1 , respectively.

• Mass Spectrometry Letters
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• v.3 no.2
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• pp.29-38
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• 2012

A new approach of volatile compounds analysis is proposed using a linear ion trap Orbitrap mass spectrometer coupled with gas chromatography through an atmospheric pressure photoionization interface. In the proposed GC-HRMS/MS approach, direct chemical composition analysis is made for the precursor ions in high resolution MS spectra and the structural identifications were made through the database search of high quality MS/MS spectra. Successful analysis of a complex perfume sample was demonstrated and compared with GC-EI-Q and GC-EI-TOF. The current approach is complementary to conventional GC-EI-MS analysis and can identify low abundance co-eluting compounds. Toluene co-sprayed as a dopant through API probe significantly enhanced ionization of certain compounds and reduced oxidation during the ionization.

• 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)

• Analytical Science and Technology
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• v.15 no.3
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• pp.221-228
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• 2002

AMX is one of extremely high mutagenic compound produced from the reaction of the chlorine and the organic compound during the disinfection of tap water. In this paper, the chemical derivatization of MX with 2% sulfuric acid-methanol, iso-propanol, sec-butanol and n-butanol derivatives for the GC/MS analysis were tested or compared. Limit of detection for the EI and NCI mode were 25 pg and 1.25 pg, respectively. The good linear calibration curve was obtained the range of 25~2500 pg by EI and NCI

• Journal of the Society of Cosmetic Scientists of Korea
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• v.25 no.3
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• pp.23-46
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• 1999

LC/MS는 HPLC의 분리능과 질량분석기의 화합물의 확인 능력을 결합시킨 기기이다. 여기서 사용되는 이온화 방법은 GCJMS에서 사용되어지는 전자이온화법(electron ionization, EI)이나, 화학이온화법(chemical ionization, CI)은 부적당하기 때문에 최근 개발되어진 연성 이온화법의 대표적인 고속원자폭격식(Fast atom bombardment, FAB)이나 전기분무이온화식 (electrospray ionization, ESI) 등이 사용되고 있다. 이중 전기분무이온화법은 고속원자폭격법에서 사용되는 매트릭스를 사용하지 않기 때문에 매트릭스 이온의 부재로 인한 낮은 바탕 신호, 오래 지속되면서 안정된 초기 이온 전류, 샘플링의 용이성, HPLC와의 더 좋은 호환성 등의 장점을 제공한다. 이러한 전기분무이온화 방법은 극성이 매우 크거나 휘발성이 낮은 물질로 보통의 EI나 CI 이온화 방법으로 분석이 어려운 물질들을 분석할 수 있다. 또한 열에 불안정하거나 분자의 분자량이 다른 단백질 등의 분석도 가능하다. 이러한 LC/ESI/MS 방법을 이용하여 열에 불안정하고 극성이면서 분자량이 커서 GC/MS 펄의 분석이 어려운 기능성 화장품 원료로 주목받고 있고 생체에 존재하는 지질 성분으로 알려진 레시틴과 세라마이드의 분석이 가능함을 소개하고 분리와 동시에 그 분자량과 구조에 대한 정보를 빠르게 얻을 수 있음을 소개하였다.

• Journal of Korean Society on Water Environment
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• v.32 no.5
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• pp.410-418
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• 2016

This study was conducted to improve the analysis method used for N-nitrosamines and to investigate the occurrences of N-nitrosamines in tributaries of the Han-river, intake stations, water treatment plants and tap water used within the city of Seoul. The samples were pretreated through a solid phase extraction and analyzed using a gas chromatography tandem mass spectrometer (GC-MS/MS). The GC-MS/MS in CI mode was compared with the GC-MS/MS in EI mode by the method detection limits (MDLs). MDLs by GC-CI/MS/MS and GC-EI/MS/MS were 0.2 ~ 1.1 ng/L and 0.2 ~ 1.4 ng/L, respectively. Samples were collected from ten tributaries of the Han-river (T1 ~ T10), six intake stations (I1 ~ I6), six water treatment plants (P1 ~ P6) and 25 taps in Seoul city. The maximum levels of N-nitrosodimethylamine (NDMA) were 0.013 μg/L, 0.008 μg/L, 0.006 μg/L and 0.002 μg/L in tributary water, raw water, finished water and tap water samples, respectively. Detected levels were much lower than 0.1 μg/L corresponding to the guideline value of WHO.

• Applied Biological Chemistry
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• v.37 no.2
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• pp.100-104
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• 1994

From the 48 hour-cultured mycelial broth of Phellinus linteus, six compounds were isolated by means of ethyl acetate extraction, silica gel column chromatography and preparative thin layer chromatography, consecutively. Compound 1 was identified as a succinic acid by the comparison of its spectral data with authentic sample. Compounds 2 and 3 were identified as p-hydroxyphenyl acetic acid methyl ester and p-hydroxybenzaldehyde by spectroscopic studies, respectively. NMR and MS studies of compound 6 revealed that it was 2,5-dihydroxymethyl furan. Compound 4, which showed similar NMR absorptions and MS fragmentation pattern with those of compound 6 was identified as 2-hydroxymethyl-5-methoxymethylfuran. These structures were verified by the spectral data of the acetate derivatives of the compounds. Compound 5 was supposed to be a N-acetyltyramine from its $^1H-NMR$ and EI-MS data, and its structure was confirmed by a synthesis starting from tyramine.

• 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.

• Journal of the Korean Chemical Society
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• v.38 no.2
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• pp.169-173
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• 1994

The previously reported cytotoxic metabolites, against the KB cell line, xestoquinone, halenaquinol sulfate and $halenaquinol^{5,6}$ were isolated from the unidentified sponge collected in October 1992, Manado Bay, Sulawesi in Indonesia. Their structure were elucidated by $^1H-,\;^{13}C$-NMR, $^1H-,\;^{13}C$(1 bond) Heteronuclear Multiple Quantum Coherence Spectroscopy$(HMQC)^1$, $^1H-,\;^{13}C$C(2 and 3 bond) Heteronuclear multiple Bond Correlation Spectroscopy$(HMBC)^2$, Electron Impact Mass Spectroscopy(EI ms), Ultraviolet Spectroscopy(UV), and Infrared Spectroscopy(IR)