• 분석과학
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• 제10권1호
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• pp.9-17
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• 1997

nitrophenol류는 미국 환경청에서 주요 priority 오염물질로 규정하고 있다. 물 중에 존재하는 nitrophenol류의 혼합물을 분석하기 위해 역상 액체크로마토그래피법에 대기압 화학이온화법을 연결한 질량분석기를 이용하였다. 추가적으로, 선택이온 검색법과 cone 전압차분해법(cone voltage fragmentation)을 이용하여 nitrophenol류의 확인에 있어서 감도와 선택성을 높였다. nitrophenol의 분해 형태는 충돌유발분해법인 MS/MS 기법으로 얻어진 분해 형태와 비교하였다.

• 대한화학회지
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• 제61권2호
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• pp.51-56
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• 2017

N-니트로사민은 이차 아민과 아질산이 산성조건 하에서 니트로소화 반응을 통해 생성되는 니트로소 화합물이다. 약 300여종이 존재하며, 그 중 90%가 동물실험을 통해 발암성이 있음이 확인되었다. 1987년 IARC에서 NDMA와 NDEA를 Group 2A로 지정하였고, NDPA, NDBA, NPYR, NPIP, NMOR을 Group 2B로 지정하였다. 본 연구에서는 N-니트로사민류의 생물학적 모니터링을 위하여 소변 중 N-니트로사민류의 분석법을 확립하였다. 소변시료는 고체상추출(Solid phase extraction, SPE)을 통하여 전처리 한 후, LC-(APCI)-MS/MS를 이용하여 정량분석 하였다. 확립된 분석법의 정확도는 85.8~110.2% 이었고, 정밀도는 1.1~10.5%로 나타났다. 검출한계는 0.0002 (NDBA) ~ 0.0793 (NDMA) ng/ml 이었고, 검량선 회귀식의 상관계수($r^2$)은 0.999 이상으로 우수한 직선성을 보여주었다. 실제 소변 중 N-니트로사민류의 평균 농도는 NDMA 2.645 mg/g creatinine, NDEA 0.067 mg/g creatinine, NMEA 0.009 mg/g creatinine, NDBA 0.011 mg/g creatinine, NPIP 0.271 mg/g creatinine, NPYR 0.413 mg/g creatinine 이고, NDPA와 NMOR은 검출되지 않았다. 추후 N-니트로사민류의 인체 노출량 평가 및 위해평가를 위한 기기분석방법으로 활용될 수 있을 것으로 판단된다.

• Journal of Pharmaceutical Investigation
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• 제33권3호
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• pp.195-199
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• 2003

The objective of this study is to investigate the pharamacokinetic parameters of decursinol following oral administration in Sprague-Dawley rats. The plasma concentration of decursinol was determined by LC/MS with APCI positive mode. The m/z value of decursinol was observed at 247. Following oral administration of decursinol extract, the apparent clearance was $5.3{\pm}2.7\;ml/hr/rat$, the absorption half life was $2.5{\pm}0.41\;hr$, the elimination half life was $3.05{\pm}1.57\;hr$, and the apparent volume of distribution was $21{\pm}12\;ml/rat$. The LC/MS method was successfully applied to the pharmacokinetic study of decursinol.

• Bulletin of the Korean Chemical Society
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• 제31권8호
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• pp.2383-2385
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• 2010

• Bulletin of the Korean Chemical Society
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• 제32권3호
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• pp.1055-1058
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• 2011

• Preventive Nutrition and Food Science
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• 제3권4호
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• pp.334-338
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• 1998

Kale(Brassica oleracea var. acephala) is one of Cruciferous vegetables that is closely related to the wild ancestral form of cabbabe. The ethanol extract of kale which contains the active compoundsss under Salmonella assay system was fractionated with chloroform to collect the nonpolar solvent soluble compounds, and then further fractionation was carried out by silica gel column chromatography. Among kale extracts separated by silical gel column chromatography, the fractions of 4, 5 and 6 exhibited strong antimutagenic activities. The major active compounds from the fraction were identified as chlorophyll derivatives by the analysis with HPLC-fritp-MS. The molecular weights of each chlorophyll derivatives in the sample were acquired from the peaks of positive ion atomosphere pressure chemical ionization (APCI) mas spectrometry.

• 분석과학
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• 제36권6호
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• pp.281-290
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• 2023

Zidovudine is an antiretroviral agent prescribed for the prevention and treatment of human immunodeficiency virus/acquired immune deficiency syndrome (HIV/AIDS). It is typically recommended to be used in combination with other antiretroviral drugs. Zidovudine has the potential to generate N-nitrosodimethylamine (NDMA) in the presence of dimethylamine and nitrite salt under acidic reaction conditions during the drug manufacturing process. NDMA is a potent human carcinogen that may be detected in drug substances or drug products. An analytical method was developed to determine NDMA in pharmaceuticals including zidovudine using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The analysis involved reversed-phase chromatography on a Kinetex F5 column with a mobile phase comprising water-acetonitrile mixtures. The detection of positively charged ions was conducted using atmospheric pressure chemical ionization (APCI). The calibration curve demonstrated excellent linearity (r = 0.9997) across the range of 1-50 ng/mL with a highly sensitive limit of detection (LOD) at 0.3 ng/mL. The developed method underwent thorough validation for specificity, linearity, accuracy, precision, robustness, and system suitability. This sensitive and specific analytical method was applied for detecting NDMA in zidovudine drug substance and its formulation currently available in the market, indicating its suitability for drug quality management purposes.

• Bulletin of the Korean Chemical Society
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• 제32권4호
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• pp.1170-1178
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• 2011

In the present study, the approach of high accuracy mass measurements for phospholipid identifications was evaluated using a 7 T ESI-FTMS/linear ion trap MS/MS. Experiments were carried out for porcine brain, bovine liver, and soybean total lipid extracts in both positive and negative ion modes. In total, 59, 55, and 18 phospholipid species were characterized in the positive ion mode for porcine brain, bovine liver, and soybean lipid extracts, respectively. Assigned lipid classes were PC, PE, PEt, PS, and SM. In the negative ion mode, PG, PS, PA, PE, and PI classes were observed. In the negative ion mode, for porcine brain, bovine liver, and soybean lipid extracts, 28, 34, and 29 species were characterized, respectively. Comparison of our results with those obtained by other groups using derivatization-LC-APCI MS and nano-RP-LC-MS/MS showed that our approach can characterize PC species as effectively as those methods could. In conclusion, we demonstrated that high accuracy mass measurements of total lipid extracts using a high resolution FTMS, particularly, 7T FTMS, plus ion-trap MS/MS are very useful in profiling lipid compositions in biological samples.

• Journal of Applied Biological Chemistry
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• 제56권1호
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• pp.43-48
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• 2013

In this study, methanol extracts from 25 indigenous Korean corals were prepared and their carotenoid constituents were analyzed by high-performance liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry (HPLC-APCI-MS). Among them, extracts from nine species showed detectable peaks in the HPLC chromatogram at 450 nm and the ultraviolet/visible spectra exhibiting carotenoid-specific characteristics were chosen. The mass data of carotenoid peaks revealed that only peridinin could be identified based on literature comparison and suggested the potential presence of novel carotenoid structures. This is the first reported investigation of indigenous Korean coral carotenoids and further work is needed to explore the carotenoids and their potential roles in the ecosystem of indigenous Korean corals.

• 농업과학연구
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• 제38권2호
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• pp.285-294
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• 2011

Glucosinolate (GSL) contents were investigated (i) at 1~7 days after sowing (DAS) in seed sprouts and (ii) at 3-7 weeks after sowing for the time-course. Moreover, (iii) They were compared with five different cultivars of rocket salad (Eruca sativa). Seventeen GSLs were separated by HPLC analysis, and 10 GSLs among them were identified as glucoraphanin, sinigrin, glucoalyssin, diglucothiobeinin, glucobrassicanapin, glucoerucin, glucobrassicin, dimeric, 4-mercaptobutyl GSL, 4-methoxy glucobrassicin, gluconasturttin by using LC-APCI-MS analysis, but 7 compounds were not identified. (i) The total GSL content in seed sprouts initially increased up to 3 DAS and then decreased according to their seedling growth. In particular, glucoraphanin known as a strong anti-cancer reagent was found the highest level (5.05 ${\mu}mol/g$ dry wt.) at 3 DAS. The most abundant GSL was glucoerucin ranged from 26.0~49.6 ${\mu}mol/g$ dry wt. (ii) In the time-course, the total GSL contents increased dramatically from 3-week (5.91 ${\mu}mol/g$ dry wt.) to 7-week after sowing (32.2 ${\mu}mol/g$ dry wt.). The major GSLs were glucoraphanin, glucoerucin and 4-methoxy glucobrassicin. (iii) By comparing GSL contents with five different cultivars, the total GSL contents increased from 4-week to 6-week after sowing, regardless of cultivar. In 4-week-old, the order with the total GSL content was "Rucola" > "Rocket Herbs" ${\geqq}$ "Odyssey" > "Takii" > "Herb", but in 6-week-old it is changed as "Takii" > "Herb" > "Odyssey" > "Rucola" > "Rocket Herbs" even there was almost no significantly difference between them.