• 한국식품과학회지
• /
• 제30권4호
• /
• pp.721-727
• /
• 1998

유기인제, 유기염소제, 카바메이트제 및 피레쓰로이드제 농약을 한 번의 전처리와 주입으로 동시에 정량 및 정성분석할수 있는 실험법을 연구하였다. 자동 soxhlet 추출 장치로 쌀시료로 부터 농약을 추출해내고, 이 추출물의 용매를 증발시킨후 hexane에 재용해하고 Sep-Pak florisil catridge를 이용한 고체상 추출법으로 정제하였다. Soxhlet 추출의 용매는 acetone을 사용하였고, 정제시의 용출용매로는 ethyl acetate-n-hexane (1:1) 혼합 용매를 사용하였다. 이와 같은 전처리 과정을 거친 시료액을 GC에 주입하고, 중간극성의 칼럼에 질량검출기를 통해 검출하였다. 이 분석법으로 쌀시료에 대해 3회의 회수율 실험을 하였을 때 captafol과 captan 등을 제외한 42종 농약이 70% 이상의 회수율을 나타내었고, 3회 반복된 실험치 간의 표준편차는 $0.29{\sim}9.07$의 범위로 나타나 비교적 양호한 재현성을 보였다.

• 한국축산식품학회지
• /
• 제29권4호
• /
• pp.482-486
• /
• 2009

The aim of this study was to optimize a simple, fast, and economical analysis procedure for the determination of 16 different pesticides in raw milk via GC/MSD. Analyses were performed via gas chromatography with electron impact mass spectrometric detection in the selected ion monitoring mode (GC/MSD-SIM) using Pentachloronitrobenzene as the internal standard. The modified sample preparation methodology was based on the Pesticide Analytical Manual (PAM) of the FDA concerning fat extraction, ACN-ether partitioning, and clean-up of the Sep-Pak florisil cartridge. The modified methodology for the determination of the 16 pesticides was validated. The range of LOQs of the 16 pesticides was likely three times lower than their Maximum Residence Levels (MRLs). The recoveries of most of the pesticides were acceptable at the fortification levels of 0.5 and 1.0 ${\mu}g/mL$ and their RSD (%) level was less than 20%. None of the 16 pesticides were detected in the selected raw milk samples.

• 분석과학
• /
• 제31권1호
• /
• pp.23-30
• /
• 2018

어린이 제품 중 22 종의 알러지 유발 방향성 물질들을 기체 크로마토그래피 불꽃 이온화 검출기(GC-FID)와 기체 크로마토그래피 질량 분석기(GC-MSD)를 사용하여 분석하였다. 분석물질들은 자동속슬렛 추출장치를 사용하여 추출하였으며, 고속 냉동 원심분리기에서 10분동안 원심분리 후 상징액을 2 mL vial 옮겨 Split mode로 주입하여 분석하였다. 확립된 조건에서 검정곡선은 0.996 이상의 상관계수를 갖는 직선성을 보였으며, 감도의 경우는 6.7~1,859,839로서 물질별로 기기특성 및 검출기에 따라 상당히 넓은 범위의 감도를 나타내었다. 기기검출한계는 $0.0032{\sim}0.0335{\mu}g/mL$로서 최대 약 $0.1{\mu}g/mL$이하의 기기검출한계를 나타내었고, 방법검출한계는 $0.0033{\sim}0.1161{\mu}g/mL$의 범위를 나타내었다. 또한 정량한계는 $0.0100{\sim}0.5422{\mu}g/mL$의 범위를 보였고, 정밀도는 0.21~4.89 %, 정확도는 89~111%의 범위를 나타내었다. 본 연구에서 개발한 분석법으로 시판품에 실제 적용하였다.

• 한국연초학회지
• /
• 제27권1호
• /
• pp.100-106
• /
• 2005

To obtain the optimum condition for analysis of 10 alkaloids in tobacco leaves, such as nicotine, nornicotine, anatabine, anabasine, myosmine, cotinine, 2,3'-dipyridyl, $\beta-nicotyrine,\;\beta-nornicotyrine\;and\;\beta-formylnornicotin$, 5 types of extraction method were investigated by GC-FID and GC/MS. The optimum condition of alkaloid extraction was achieved by using methanol:dichloromethane(1:3, v/v) after NaOH treatment. The use of mass selective detector (MSD) provided unambiguous nicotine related alkaloid analysis. Alkaloids in various tobacco leaves were extracted with the optimum extraction condition and quantified by GC/MS/SIM mode. Compared with concentrations of alkaloids among the various tobacco leaves, the concentration of alkaloids was generally in the order burley > flue-cured > oriental tobacco. In flue-cured tobacco leaves, the order of concentration of alkaloids was nicotine > anatabine > nornicotine > $\beta-nicotyrine\;>\;\beta-formylnornicotine\; >\;myosmine\;>\;2,3'-dipyridyl\;>\;cotinine\;>\;anabasine\;>\;\beta-nornicotyrine$. However, in the case of burley and oriental tobacco leaves, the concentration of nornicotine was higher than that of anatabine.

• 한국응용과학기술학회지
• /
• 제28권1호
• /
• pp.64-74
• /
• 2011

The aim of study was to investigate polluted amounts 16 PAHs in railroad(waste railway ties) area, factory area and land-fill area. All of the samples were analyzed by GC-MSD(SIM mode), and the recovery range, detection limit and standard deviation obtained by this experiment were 73.88 ~ 94.75%, 0.009 ~ 2.252 ${\mu}g$/kg and 1.861 ~ 12.373, respectively. The concentrations of total PAHs(t-PAHs) and total carcinogenic PAHs(t-PAHcarc) in soils of three area were in the range of 12.54 ~ 3274.95 ${\mu}g$/kg on a wet weight basis with a mean value of 499.8 ${\mu}g$/kg and 0 ~122.77 ${\mu}g$/kg with a mean value of 20.16 ${\mu}g$/kg, respectively. The correlation between t-PAHs and t-PAHcarc appeared very high in railroad(waste railway ties) area ($R^2$ = 0.8301), factory area ($R^2$ = 0.9217) except land-fill area($R^2$ = 0.3782), indicated that t-PAHcarc concentration increases in proportion with t-PAHs.

• 분석과학
• /
• 제22권2호
• /
• pp.119-127
• /
• 2009

폐기물공정시험법과 내분비계 장애물질 시험방법을 이용하여 사업장폐기물소각재 24건 및 생활 쓰레기소각재 20건에 대하여 잔류성 유기오염물질의 분포특성을 확인하였다. 12종류의 잔류성 유기오염 물질중에서 7종을 GC-MSD (SIM-mode)로 정량분석을 하였다. 총 44건의 시료 중 21 시료에서 헥사클로로벤젠이 검출되었으며, 나머지는 모두 불검출이었다. 헥사클로로벤젠은 사업장폐기물의 소각재에서는 0.132-8.138 ng/g, 비산재에서는 0.195-5.765 ng/g, 그리고 생활쓰레기 소각장의 소각재에서는 0.270-1.828 ng/g, 비산재에서는 0.154-50.643 ng/g 정도로 각각 검출되었다.

• 한국식품위생안전성학회지
• /
• 제5권3호
• /
• pp.159-164
• /
• 1990

To detect and quantitation residual antibiotics and antibacterial agents in meats, we performed a biological assay employing the three microorganisms Bacillus subtilis ATCC 6633, Micrococcus luteus ATCC 9341, and Bacillus cereus var. mycoides ATCC 11778 for the screening purpose and developed a Gas Chromatography-mass Spectrometry(GC/MS) analysis for the confirmation and quantiation. In the biological assay (paper disk method), three test solution are used depending on the character of the residual antibiotics and antibacterial agents, follow by a simple clean up procedure which includes homogenization with Mcilvaine buffer, defatting with includes homogenization with Mcilvaine buffer, defatting with hexane, extraction with chloroform, clean-up by Sep-Pak $C_{18}$ and Bakerbond SPE carboxylic acid column. The chloroform layer is used for the analysis of sulfa agents. macrolides antibiotics and antibacterial agents, Adsorbed materials in the Sep-Pak $C_{18}$ were also employed for th analysis of penicillins and tetracyclines. Effluents from the Sep-Pak $C_{18}$ were cleaned-up one more by Bakerbond 10 SPE COOH column and employed for the analysis of aminoglycosides. In the instrumental analysis by using the GC/MSD, residual antibiotics and antibacterial agent were quantitated by selected ion monitoring (SIM) mode after derivatization. A simultaneous analysis of six residual antibiotic and antibacterial agent such as oxytetracycline, penicillin, ampicillin, choliraphenicol and thiamphenicol was developed with simple cleanup procedures revealing good recovery and reproducibility. Also, simultaneous detection of macrolides antibiotics such as erythromycin, spiramycin, and oleandomycin was developed after acid hydrolysis due to their large molecular structures. Because of the high reproducibility and selectivity of these two methods, it is very desirable that the combination of the two methods be used in the bioassay for the screening of residual antibiotics and antibacterial agent and that GC/MSD analysis be used for the confirmation and quantitation.

• 한국환경과학회지
• /
• 제15권7호
• /
• pp.669-676
• /
• 2006

PAHs are major pollutants that are widely distributed in soil and groundwater environment, so that may be regarded as carcinogens. We investigated the degradation kinetics of PAH in aqueous solution when low pressure UV energy and ultrasonic irradiation were applied. Phenanthrene and pyrene were used as model compounds. The degrees of degradation of these compounds with time were analyzed with a GC/MSD (SIM-mode). UV photolysis experiments showed that phenanthrene was reduced by 90 -67% at initial concentrations of 1 ppm to 8ppm whilst it decreased to 50% at 10 ppm. Under the same conditions pyrene was degraded up to about 75% at lower initial concentrations but the reduction efficiency dropped to a level of 34 to 29% at the higher concentrations above 8 ppm. The reaction orders for phenanthrene and pyrene were found to be zero-th and ca. -0.4th order, respectively, thus implying that the reported assumption of pseudo 1st order reaction for some PAHs would be no longer valid. PAH degradation was roughly proportional to the intensity of UV (number of lamps), exhibiting maximum 92.5% of the degradation efficiency. The solution pH was lowered to 4.4 from 6.4 during the experiments partially because the carbons decomposed by the energy reacted with oxygen radicals to produce carbon dioxides. Ultrasonic irradiation on phenanthrene solutions gave relatively poor results which matched to 50 to 70% of degradation efficiency even at 2 ppm of initial concentration. Phenanthrene was found to be degraded more efficiently than pyrene for the two energy sources. Ultrasound also followed the same reaction kinetics as UV energy on PAH degradation.

• 분석과학
• /
• 제27권6호
• /
• pp.339-346
• /
• 2014

근로자 건강진단 실무지침 상의 필수 검사항목 항목 중, N-메틸아세트아미드의 소변 표준시료를 제조하여 그 신뢰도를 확인하고자 하였다. DB-624 컬럼을 사용한 GC/MSD 분석 방법에 의해 기존 분석 컬럼보다 우수한 분리능과 선택성으로 N-메틸아세트아미드를 분석하였다. -60, -20, 5, $25^{\circ}C$에서 5-50 mg/L의 농도 범위의 소변 중 N-메틸아세트아미드의 안정성을 6개월 보관 시점까지 검토한 결과 모든 보관 조건에서 안정하였으며, 각 시료에 대한 균질성 검사 결과도 양호하였다. 이상의 결과로부터 유리형 NMAC를 첨가하는 방법으로 제조한 소변 중 NMAC 표준시료가 분석정도관리용으로 실용화하기에 적합한 균질성과 장기간 보관 시의 안정성을 모두 만족시킴을 확인하였고, 2008년부터 분석정도관리 표준시료로 활용하였다.

• 분석과학
• /
• 제23권2호
• /
• pp.187-195
• /
• 2010

허베이 스피리트호 유류유출 사고 후 지역주민들의 수산물 섭취로 인한 건강 위해도를 평가하기 위하여, 가스크로마토그래피-질량분석기(GC-MSD)를 이용하여 유류유출 지역 주민들이 직접 채취 및 구입한 수산물 중 다환방향족탄화수소류(PAHs) 16종을 분석하였다. 시료는 KOH로 가수분해하여 Methylene chloride로 추출하였다. 추출액 중의 16개의 PAHs는 실리카/플로리실 정제컬럼을 이용하여 Methylene chloride : n-헥산(1:9) 혼합용액으로 용출하였고 GC-MSD의 SIM을 이용하여 분석하였다. 16 개의 PAHs의 평균 회수율은 79~85%이었으며, 126개의 시료에서 $0.17\sim6.04\;{\mu}g/kg$ 수준으로 검출되었고, Benzo(a)pyrene의 독성등가계수(TEF)를 적용한 Benzo(a)pyrene 독성등가량($TEQ_{BaP}$)은 $0\sim0.91\;{\mu}gTEQ$/kg 수준이었다. 또한 유류유출 지역 주민들의 벤조피렌의 일일 평균 노출량은 $5.5{\times}10^{-8}\;mg/kg$ bw/day 이었고, PAHs 일일 평균 만성노출량은 $1.3{\times}10^{-5}\;mgTEQ$/kg bw/day이었다. 그리고 안전마진(MOE)과 초과발암위해도는 각각 $1.8{\times}10^6$, $9.8{\times}10^{-8}$으로 사람에게 위해영향발생 우려가 낮은 수준이었다.