• 한국지하수토양환경학회지:지하수토양환경
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• 제17권3호
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• pp.1-9
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• 2012

According to the agreement on WTO/TBT, we are under the situation to adopt international standard (ISO standard) as a national standard if it exists. However, in case of environmental area, it is a domestic legal obligation to use Korean environmental standard method(KESM) for analyzing various contaminants. Therefore it is necessary to assess the comparability between KEM and ISO standard prior to apply ISO standard to soil conservation law in Korea. The main purpose of this study is to assess the comparability of both methods for analyzing heavy metals in soil. We looked over various aspects like pre-treatment, calibration curve range, detection wavelength, soil organic matter content and so on. Apparently, the procedure of both methods is almost same. However in details, both methods are different in stationary time before aqua-regia extraction using reflux system, calibration curve range for Cu, Pb, Ni and measuring wavelength for Pb. According to the results of comparison test, the results were significantly different when the different calibration range was used. In case that all the extracts independent of methods were reanalyzed with the same calibration range of each method, both methods showed statistically same results. Other conditions like different stationary time, measuring wavelength of AAS and soil organic matter content did not have any influence on the analytical result. Therefore, we suggest to extend the calibration curve range to 0~8 mg/L which is used in KS I ISO standard(Korean standard related with environment which is translation version of ISO standard without any technical change). In case of $Cr^{6+}$, the results showed no significant differences between two methods even though the pretreatment, instrumentation and other analysis conditions were different. In addition to UV/Visble spectrometry of KESM for soil contamination, we suggest to adopt ion chromatography of ISO 15192(US EPA method 7199) for analyzing $Cr^{6+}$ with the consideration of laboratory work efficiency.

• 생명과학회지
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• 제24권8호
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• pp.860-864
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• 2014

별불가사리(Asterina pectinifera)의 유문 맹낭 추출물로부터 새로운 항균활성 펩타이드를 정제하기 위해서 유문 맹낭 추출물을 역상 HPLC와 이온 HPLC column에 주입하였다. 강한 항균활성을 나타내는 2개의 새로운 펩타이드가 유문 맹낭 추출물로부터 정제되었다. 이러한 물질들은 Pyloric caeca Asterina pectinifera peptides (PAP-1와 PAP-2)라 명명하였다. 정제한 물질들의 특성을 알아보기 위해서, 분자량 및 아미노산 서열 분석은 MALDI-TOF 질량분석기와 에드만 분해법으로 조사하였다. PAP-1과 PAP-2의 분자량은 각각 약 2952 Da 및 2980 Da이었다. PAP-1과 PAP-2의 부분적인 N-말단 서열은 다음과 같다. PAP-1, AIQNAGES; PAP-2, AIQNAAES. PAP-2는 PAP-1의 6번째 위치(glycine or alanine)에서 한 잔기만 다른 isoform에 해당된다. 지금까지 밝혀진 항균활성 펩타이드와의 분자량 및 N-말단 아미노산 서열을 비교한 결과, 이들 물질들은 다른 물질들과 동일성을 나타내지 않았다. 이러한 발견은 PAP-1과 PAP-2가 별불가사리의 유문맹낭의 선천성 방어계에 중요한 역할을 담당하고 있는 것을 시사하고 있다.

• 분석과학
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• 제32권2호
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• pp.35-47
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• 2019

In this study, high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was employed to detect 26 antidiabetic compounds in adulterated dietary supplements using a simple, selective method. The work presented herein may help prevent incidents related to food adulteration and restrict the illegal food market. The best separation was obtained on a Shiseido Capcell Pak(R) C18 MG-II ($2.0mm{\times}100mm$, $3{\mu}m$), which improved the peak shape and MS detection sensitivity of the target compounds. A gradient elution system composed of 0.1 % (v/v) formic acid in distilled water and methanol at a flow rate of 0.3 mL/min for 18 min was utilized. A triple quadrupole mass spectrometer with an electrospray ionization source operated in the positive or negative mode was employed as the detector. The developed method was validated as follows: specificity was confirmed in the multiple reaction monitoring mode using the precursor and product ion pairs. For solid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL, and for liquid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL. Satisfactory linearity was obtained from calibration curves, with $R^2$ > 0.99. Both intra and inter-day precision were less than 13.19 %. Accuracies ranged from 80.69 to 118.81 % (intra/inter-day), with a stability of less than 14.88 %. Mean recovery was found to be 80.6-119.0 % and less than 13.4 % RSD. Using the validated method, glibenclamide and pioglitazone were simultaneously determined in one capsule at concentrations of 1.52 and 0.53 mg (per capsule), respectively.

• 한국식품위생안전성학회지
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• 제25권4호
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• pp.388-394
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• 2010

Metabolomics aims at the comprehensive, qualitative and quantitative analysis of wide arrays of endogenous metabolites in biological samples. It has shown particular promise in the area of toxicology and drug development, functional genomics, system biology and clinical diagnosis. In this study, analytical technique of MS instrument with high resolution mass measurement, such as time-of-flight (TOF) was validated for the purpose of investigation of amino acids, sugars and fatty acids. Rat urine and serum samples were extracted by selected each solvent (50% acetonitrile, 100% acetonitrile, acetone, methanol, water, ether) extraction method. We determined the optimized liquid chromatography/time-of-flight mass spectrometry (LC/TOFMS) system and selected appropriated columns, mobile phases, fragment energy and collision energy, which could search 17 metabolites. The spectral data collected from LC/TOFMS were tested by ANOVA. Obtained with the use of LC/TOFMS technique, our results indicated that (1) MS and MS/MS parameters were optimized and most abundant product ion of each metabolite were selected to be monitorized; (2) with design of experiment analysis, methanol yielded the optimal extraction efficiency. Therefore, the results of this study are expected to be useful in the endogenous metabolite fields according to validated SOP for endogenous amino acids, sugars and fatty acids.

• 대한원격탐사학회지
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• 제36권6_3호
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• pp.1669-1679
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• 2020

본 연구는 강우 강도에 따른 대기 중 미세먼지(particulate matter, PM) 저감효과와 미세먼지를 구성하는 주요 수용성 이온에 의한 빗물 수질(pH, 전기전도도(electrical conductivity, EC), 수용성 이온 농도) 변화를 평가하였다. 2020년 3월부터 7월까지 총 6번의 강우를 대상으로 부산 부경대학교 캠퍼스에 집수장치를 설치하여 pH와 EC를 실시간 측정하였으며, 강우의 양이온(Na+, Mg2+, K+, Ca2+, NH4+) 및 음이온(Cl-, NO3-, SO42-)의 농도는 이온크로마토그래피(ion chromatography, IC)를 이용하여 분석하였다. PM10 농도는 강우 전후로 자체제작한 미세먼지 센서를 이용하여 실시간으로 측정하였다. 총 282개의 빗물 샘플의 수질을 분석한 결과, 초기 강우의 pH는 평균 4.3으로 산성도가 높았으며, EC는 평균 81.9 μS/cm으로 평균 NO3- (5.4 mg/L), Ca2+ (4.2 mg/L), Cl-(4.1 mg/L)의 농도가 높게 검출되었다. 그리고 강우가 지속됨에 따라 pH는 증가하는 경향을 보였으며 EC는 상대적으로 감소하는 경향을 보였다. 강우 강도가 7.5 mm/h 이상(heavy rain)일 때 대기 중 평균 60% 이상의 PM10 농도 저감효율을 보였으며, 강우 강도 5 mm/h 이하(light rain)일 때 평균 40% 이하의 저감효율이 나타났다. 빗물 수질 분석 결과, 강우 강도가 증가할수록 초기 강우의 산성도와 EC가 증가하는 경향을 보였으며 초기 강우 내 이온 농도 또한 높은 농도로 검출되었다. 이는 대기 중 PM10이 초기의 강도 높은 강우에 따른 저감효과에 상당한 영향을 받는 것으로 판단된다.