• 분석과학
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• 제17권4호
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• pp.322-336
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• 2004

항암치료제인 tamoxifen을 복용한 후 체내에서 분비되는 tamoxifen과 그 대사체를 trifluoroacetic anhydride (TFAA), pentafluoropropionic anhydride (PFPA), 및 heptafluorobutyric anhydride (HFBA) 유도체화 시약으로 이들이 함유하고 있는 히드록시기를 아실화반응시킴으로써 기체크로마토그래피와 질량분석기로 분석 가능하게 하고, 검출한계 등을 개선한 새로운 방법에 대해 연구하였다. 한편 질량 분석기로 검출하기 위한 이온화 방법의 하나인 전자 충격 이온화법과 화학 이온화법을 비교하여 보다 개선된 분석법을 연구하고, 이 방법을 실제 인체 뇨시료에 적용한 tamoxifen 대사체 검출을 위한 최적 조건을 연구하였다. Acylation 방법에 있어서의 최적 반응조건은 반응 온도 $50^{\circ}C$와 반응 시간 30 min 이었으며, 뇨시료에 있어서 tamoxifen 대사체 추출에 대한 최적 pH는 7.0, 추출 용매는 디에틸에테르가 적절함을 알 수 있었다. TFAA, PFPA, HFBA로 유도체 시킨 후 CI법과 EI법을 비교 분석한 결과, NCI법에서는 주로 $[M-HF]^-$ 또는 $[M-2HF]^-$이온이 주요 이온으로 나타났으며 NCI에서 감도가 뛰어난 할로겐원소가 함유된 유도체 시약을 사용하였기 때문에 생체시료 내에 미량 존재하는 약물을 보다 용이하게 검출 및 확인 할 수 있었다. 한편 GC/MS로 tamoxifen대사체를 분석한 결과 tamoxifen이 간에서 대사 될 때 주 대사체로 알려져 있는 4-hydroxytamoxifen은 검출 되지 않았고 hydroxymethoxytamoxifen이 주 대사체로 검출되었다. Acylation 유도체화 과정을 거친 hydroxymethoxytamoxifen은 NCI에서의 토막 이온을 조사한 결과 아미노 그룹의 ${\beta}$-cleavage가 일어난 m/z 491이온, acylation 유도체 한 분자가 쪼개진 m/z 344이온이 비교적 높게 검출되었다.

• 한국물환경학회지
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• 제37권6호
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• pp.510-519
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• 2021

Volatile Organic Compounds (VOCs) in sediments, which can cause human health problems, have been monitored in Korea since 2014. Measured VOC concentrations can be affected by matrix type and the volatility of target substances. In this study, (1) VOCs volatility and the influence of matrix interference were confirmed, and (2) internal standards (IS) method was applied to improve analytical method. For these purposes, method detection limit (MDL), calibration linearity, precision and accuracy of VOCs were compared in various matrices using the IS. Some of VOCs in sediments showed different peak areas and reduced rates compared to water matrix. It was suggested that adsorption properties of sediments hindered the migration to vapor during heat pretreatment in headspace method. A calibration curve was created in clean sand. Recovery rates for the calibration curve method and IS applying method were 64.1~83.1% and 99.1~119.3%, respectively. Relative standard deviations ranged from 11.1% to 21.6% for the calibration curve method and those for IS ranged 4.7% to 13.7%. In case of real sediment, calibration curve and 1,2-Dichlorobenzene-d4 (ODCB) among IS were not suitable. The average recovery rate of Fluorobenzene (FBZ) increased by 56.4% and Relative Standard Deviation (RSD) by 4.7%. However, the recovery rate was increased in the samples with large values of igniting intensity. This study confirmed that influence of the matrix of VOCs in sediment, and addition of IS materials improved precision and accuracy. Although IS corrects volatilization and adsorption, it is recommended that more than two types of IS should be added rather than single.

• 현장농수산연구지
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• 제23권1호
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• pp.5-12
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• 2021

꽃향유에 함유된 정유를 추출하기 위해 개화한 개체를 채집한 후 생체를 실험에 이용하였다. 재료는 꽃 0.7kg, 잎 + 줄기 1.5kg으로 나누어 부위별로 추출 후 향기패턴 분석에 사용하였고, 정유성분 분석을 위해 전초 5kg을 넣은 후 추출하였다. 정유추출은 Schultz등(1977)이 개량한 SDE 법으로 정유를 추출하였으며, 추출시간은 시료가 끓기 시작한 후부터 1시간으로 하였다. 이렇게 추출한 정유성분을 전자코를 이용하여 향기패턴 분석과 GC-MS로 정유성분의 물질을 분석하였던 결과는 다음과 같다. 1. 향기패턴 분석은 꽃에서 추출한 정유성분의 경우 10~20분에 나오는 향의 질이 가장 좋았고 줄기와 잎에서 추출한 향은 다소 향의 질은 좋지 못했지만 10~40분에 나오는 향이 좋았다. 향의 세기는 꽃만으로 추출한 것은 10~20분에서 가장 강한 향이 나왔고, 30~40분에서도 향의 세기는 높게 나타났다. 줄기와 잎에서 추출한 향은 대체로 향의 세기가 강하지 못하였지만 10~20분에서 높게 나타났다. 2. 꽃향유에 함유된 정유의 종류는 40종을 얻었다. 이중 Mequinol, Benzene, 1,2,3,4-tetramethyl, Elsholtziaketone, Dehydroelsholtziaketone을 확인하였다.

• 분석과학
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• 제18권5호
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• pp.444-451
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• 2005

참기름에서 스테롤류와 지방산을 간편하고 정확하게 추출하는 방법을 개발하였다. 새로운 방법은 특히 세사민의 추출 효율을 크게 향상하여 세사민과 캄파스테롤의 비율을 크게 향상시켜 감정의 도구로 응용이 가능할 것으로 판단되었다. 또 기타 스테롤류도 확인하였다. 유도체화를 진행시키면 지방산과 스테롤류의 동시 분석이 가능하였으나, 감정의 도구로는 더 많은 실험이 필요할 것으로 판단되었다.

• 한국산업보건학회지
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• 제23권3호
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• pp.222-228
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• 2013

Objectives: The indoor air quality of newly-built (NC) and remodeled (RC) school classrooms was assessed. The primary aim was to show correlations between volatile organic compounds (VOCs) and formaldehyde (HCHO) pollutant levels. Methods: This study investigated the indoor air concentrations of VOCs and HCHO at 26 sites of newly built and 68 sites of remodeled classrooms located in South Gyeongsang Province between 2010 and 2012. VOCs in the indoor air were determined by adsorbent tube (Tenax TA) and automatic thermal desorption coupled with GC-MS analysis. Target analytes were five VOCs: benzene, toluene, ethylbenzene, xylene, and styrene. HCHO was collected with a 2,4-DNPH cartridge and analyzed by HPLC. Conclusions: This study estimated that indoor VOCs and HCHO concentrations in the classrooms were mainly affected by interior building materials and classroom equipment. For proper indoor air quality in schools, classroom air should be improved through reduction of hazardous materials by adequate ventilation, selecting environmental friendly materials, etc.

• Environmental Engineering Research
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• 제12권3호
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• pp.93-100
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• 2007

I improved an analytical method for determining trace amounts of eleven phenolic endocrine-disrupting chemicals (11 phenolic EOCs) in human urine. The 11 phenolic EOCs were subjected to hydrolysis and then to solid phase extraction with a XAD-4 column. Alkylphenols, chlorophenols, and bisphenol A in XAD-4 column were eluted with acetonitrile, and the eluate was concentrated under a nitrogen stream, and then tert-butyldimethylsilylation. Separation and determination were done by gas chromatography, using mass spectrometry operating in the selective ion monitoring mode for quantitation. For tert-butyldimethylsily (TBDMS) derivatization the recoveries were $91.2{\sim}125.9%$, the limits of quantitation (LOQ) for the 11 phenolic EOCs in the nanogram-per-milliliter range ($0.025{\sim}1.000\;ng/mL$) were thus achieved by using 1 mL of urine, and the SIM responses were linear with the correlation coefficient varying by $0.9300{\sim}0.9943$. Based on the results for urine samples from unexposed individuals, 4-tert-octylphenol and pentachlorophenol were detected in hydrolysed urine sample. Other alkylphenols, chlorophenols and bisphenol A were not detected.

• 한국자원식물학회:학술대회논문집
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• 한국자원식물학회 2020년도 추계국제학술대회
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• pp.78-78
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• 2020

Cruciferous plants such as broccoli and radish contain glucosinolate, which is a bioactive precursor that is most often used in Korean foods and is unique as a food ingredient. In addition, it contains various other phytochemicals and is promising as a health-oriented food material. In particular, Sulforaphane is a hydrolyzate of the glucosinolate, which has a more beneficial effect on the human body. Glucosinolate may be hydrolyzed by enzymes called myrosinase, which is voluntarily possessed by cruciferous plants. However, the ESP(Epithiospecifier protein) in broccoli sprouts could acts competitively with myrosinase, and convert to the less bioactive sulforaphane nitrile form. Therefore, we improved the yielding of sulforaphane in broccoli sprouts with a new method. We induce inactivation of the ESP protein by heat treatment. At this time, a myrosinase was introduced from the radish sprout because myrosinase in broccoli sprouts is also denatured by heat treatment. According to the results, we have confirmed by GC / MS that formation of sulforaphane increases more than 7 fold using set heating and mixing conditions.

• 한국의류학회지
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• 제35권2호
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• pp.218-229
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• 2011

Dyeing properties of cotton and ramie fabrics with pine needles colorants were studied by investigating the analysis of pine needles colorants, the effect of dyeing conditions (such as dye concentration, dyeing temperatures and times on dye uptakes), effect of mordants, and color change. The various colorfastness of dyed fabrics were evaluated for practical use; in addition, the antimicrobial ability, ultraviolet-cut ability, and deodorant ability were estimated. In the UV-Visible spectrum, the wavelength of the maximum absorption for pine needles extract was 285nm, and pine needles colorants produced a yellow color. From FT-IR and GC-MS results, it was assumed that chromophoric substance from pine needles extracts were mixed with flavonol tannin and flavanol tannin. An increased dyeing concentration resulted in a larger dye uptake and a Freundlich absorption isotherm was obtained. A larger dye uptake occurred as the dyeing time and temperature increased. Post-mordanting was more effective than pre-mordanting and the dye uptake of fabrics improved by mordanting. The colorfastness of dyed fabrics showed a low rating; however, colorfastness to washing and dry cleaning of cotton fabrics mordanted with N.Cu, and friction fastness of ramie fabric mordanted with Cu improved. The dyed fabrics showed very good antimicrobial abilities of 99.9%. In addition, the ultraviolet-cut ability and deodorant ability improved in fabrics dyed with pine needles extracts.

• 한국환경농학회지
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• 제32권3호
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• pp.214-223
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• 2013

Dichlorprop(DCPP)는 phenoxyalkanoic acid계열로서 인체에 유해한 것으로 알려진 fenoprop, 2,4-D 및 daminozide의 대체 약제로 사용되어온 auxin 활성 생장조정제로 과수의 낙과 방지에 이용된다. 하지만, DCPP의 과다 사용은 과실의 숙기를 촉진시키며 연화 및 저장력을 현저히 저하하는 부정적인 영향을 나타내며, 제초제의 특성을 나타내기 때문에 농산물에 과다 사용하여 잔류허용기준을 초과할 경우, 인체에 유해할 수 있다. 따라서 본 연구는 생장조정제로 사용되고 있는 DCPP에 대하여 국내에 유통되는 농산물을 대상으로 잔류 실태 조사 연구를 실시하고자 기존 식품공전 분석법을 개선하여 신속하고 효율적인 분석법으로 재확립 하였다. 분석법 검증에 사용된 시료는 농산물의 메트릭스를 대표할 수 있는 농산물 5종(감귤, 감자, 고추, 대두 및 현미)을 사용하였다. 검체에 아세톤을 가하고 산성화시켜 추출한 후 산-염기 액-액 분배법을 이용해 추출, 정제 및 농축 과정을 거쳤다. 농축에 의해 얻어진 잔류물은 메탄올로 재용해한 후, 이중 2 mL를 취해 $BF_3$-메탄올 용액으로 메틸화한 후, 헥산 및 5% 염화나트륨을 사용해 최종 정제를 거친 용액을 헥산으로 재용해하여 GC/ECD에 주입하였다. 기기분석은 DB-17 중간 극성 칼럼과 운반 기체로 질소 가스를 사용하였고, split-less 모드 하에 $1{\mu}L$를 주입하여 승온 조건으로 ECD에 의해 측정하였다. 또한, GC/MS를 통해 확인시험을 수행 하였으며, 모든 검증은 CAC 가이드라인(CAC/GL 40, 1993) 규정에 따라 실시하였다. 그 결과, DCPP의 정량 한계는 모든 검체에서 0.05 mg/kg 수준이었고, 회수율은 감귤89.5-94.3%, 감자 79.4-87.4%, 고추 90.5-102.2%, 대두 78.8-101.1%, 현미 90.5-100.4%였으며, 변동계수는 감귤 2.5-9.5%, 감자 1.4-2.6%, 고추 2.7-3.9%, 대두 3.4-7.3%, 현 미 1.2-2.1%로 나타났다. 이상의 결과는 국제식품규격위원회 가이드라인 규정(CAC/GL 40, 1993)에 만족하는 수준으로, 새롭게 개선된 DCPP 분석법은 향후 국내 유통 농산물을 대상으로 한 생장조정제 DCPP의 잔류 실태 조사 연구에 활용될 계획이다.

• 한국대기환경학회지
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• 제30권6호
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• pp.586-599
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• 2014

During the last two decades, indoor air quality and volatile organic compounds (VOCs) have been of concern in Korean society due to their nature of potential health impacts. In order to investigate the pollution levels of VOCss in indoor environments, establishment of a solid test method for monitoring the airborne VOCss is essential. In Korea, a method based on adsorbent sampling and GC analysis coupled with thermal desorption was proclaimed as the Korea Standard Method for Indoor Air Quality Test. This study was carried out to examine some inherent problems of the VOCs measurement method. The VOCs method does not describe in detail preparing the standard samples. The standard samples may be prepared by impregnation of either liquid standard solutions or a mixture of standard gases. In this study, we investigated the optimal temperature condition for transferring the liquid standards onto a standard adsorbent tube. As a result, keeping the impregnation temperature at $250^{\circ}C$ will be recommended in regard of the boiling points of multiple target analytes and the thermal stability of the adsorbent. We also demonstrated some problems associated with handling of a syringe used for transferring the standard solutions onto the adsorbent tubes, and a best way to get rid of the syringe problems was suggested. Finally, a number of field works were conducted to evaluate the performance of adsorbent sampling methods. Comparison of different adsorbent tubes, i.e. tube packed with single sorbent (Tenax) and double sorbents (Tenax with Carbotrap), revealed that 30 to 40% differences between the two groups, implying that sampling efficiency is depending on the volatility and the strength of adsorbents. However, duplicate precisions for VOCs sampling with a same type of adsorbent and at same flow rates appeared to be satisfactory to be all within 20%, which is a quality control guideline. Distributed volume precisions were also found to be within a guideline value, 25%, although the precision was in general inferior to the duplicate precision. The Korea indoor VOCs test method should be more refined and improved in many aspects, particularly procedure and instrumentation for preparing the standard samples and specification of quality control assessment.