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고분해능 질량분석장치를 이용한 수중 피레스로이드계 농약성분 동시분석
최재원 ( Jae Won Choi ),김윤석 ( Yun Seok Kim ) 한국환경분석학회 2011 환경분석과 독성보건 Vol.14 No.1
A gas chromatography-high resolution mass spectrometry (GC-HRMS) method with solid-phase extraction has been developed to simultaneously quantitate pyrethroid pesticides in water samples. Target compounds in this study were permethrin, cypermethrin, fenpropathrin, cyhalothrin(-l, -g), cyfluthrin, tefluthrin, flucythrinate and bifenthrin. To improve sensitivities of the method for pyrethroid pesticides, framgment ions were surveyed to select a quantification mass with the second prior mass or molecular mass as a qualificator. Deuterium poly aromatic hydrocarbons like phenanthrene-d10 and perylene-d12 were added as a internal standards. Prior to sample analysis, disk type solid-phase extraction was validated using RPS and C18 for raw and treated water. Higher average recoveries ranged from 80% to 87% were observed in C18 disk for raw and treated water. Performance test of SPE-GC-HRMS method for pyrethroid pesticides were carried out with samples spiked with target compounds at 5 ng/L each. Method detection limits (MDLs) were 0.90~7.45 ng/L with the accuracy of 71~98% and the precision of 7.2~10.4% exept for cypermethrin(21.8%). The developed method was applied to quantitate the residual pesticides in river water (n=3), surface water from apple farm (n=2) and tap water (n=5). Target compounds were not detected from all samples, but interfering peaks caused by similar fragments with different retention times were observed.
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HPLC/ESI-MS/MS를 이용한 환경 시료중 Estrogens의 분석
서천규 ( Cheon Kyu Seo ),명승운 ( Seung Woon Myung ) 한국환경분석학회 2010 환경분석과 독성보건 Vol.13 No.3
Trace concentrations of estrogens such as 17β-estradiol (E2), 17α-estradiol (αE2), estrone (E1), estriol (E3), and 17α-ethinylestradiol (EE2) may have adverse effects on humans and the aquatic ecosystem. The environmental analysis of estrogens at physiologically active concentrations (low ng/L) requires the use of very sensitive and selective method. An analytical procedure for the simultaneous determination of five steroid estrogens in an aqueous environmental sample is described. The procedure includes solid phase extraction/clean-up with C18 cartridge, and analysis by liquid chromatography/tan dem mass spectrometry of five estrogens. After 500 mL of sample loading on C18 cartridge, sample was eluted with acetonitrile and dryness. The reconstituted analytes were separated on HPLC system with 0.1% formic acid and acetonitrile followed by analyzed using (-) electrospray ionization-mass spectrometer with multiple reaction monitoring mode. In the range of 0.05-1 ng/mL, the calibration curves were showed the good linearities (above r2=0.99). The limits of detection and limits of quatitation estimated for the estrogens in blank surface water were the concentration range of 0.055~0.154 ng/mL and 0.184~0.514 ng/mL, respectively. The absolute recovery, precision (intra-day) and accuracy in the low, medium and high (0.005~1.0 ng/mL) were in the range of 69.5~95.1%, 0.4~7.9% (RSD) and -9.1~9.3% (bias), respectively.
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의암호 남조류 발생 제어를 위한 수질 장기모니터링 및 환경요인 분석
이석종 ( Seog-jong Lee ),임병찬 ( Byung-chan Lim ),이건호 ( Geon-ho Lee ),정원구 ( Won-gu Jeong ),허범녕 ( Beom-nyung Hur ),허인량 ( In-ryang Hur ) 한국환경분석학회 2016 환경분석과 독성보건 Vol.19 No.2
We monitored the water quality and algal communities to analyze the environmental factors that contributed to the development of cyanobacterial blooms in lake Uiam from 2012 to 2015. Anabaena species were isolated as the dominant type of cyanobacteria in the lake, and these were first observed at sites S6~S9 from June to July. The total phosphorus (T-P) concentration was estimated at 0.015 mg/L in 2015 and 0.043 mg/L in 2011, which represents a reduction of 65%. Hence, the N/P ratios in the lake also changed, i.e., the ratios were 110~130 in 2014~2015, and 40~70 in 2010~2013. The daily loads of T-P were reduced 5.3 kg/d and 8.8 kg/ d in 2014 and 2015, respectively, which were better loading rates than the value of 23.0 kg/d and 16.6 kg/d in 2012 and 2013, respectively. Algae blooms did not occur in Lake Uiam during 2014 to 2015. According to our analysis of critical environmental conditions, blooms will readily occur when N/P ratios are 20~30 and water temperatures are maintained at 20~25°C over a period of 30 days; moreover, 50~60 mm of precipitation is needed from the middle of June to early July.
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액체크로마토그래피-텐덤질량분석법에 의한 하천수 및 정수 중 남조류 기원 신종 독소 BMAA(β-N-Methylamino-L-Alanine)의 정량분석
최재원 ( Jae-won Choi ),장제헌 ( Jae-heon Jang ),김애경 ( Ae-kyung Kim ),이선홍 ( Sun-hong Lee ) 한국환경분석학회 2021 환경분석과 독성보건 Vol.24 No.4
β-Methylamino-L-alanine(BMAA)isanemergingalgaltoxinthathasdrawnattentionbecauseitcancauseneurodegenerativediseases,includingParkinson'sdiseaseandAlzheimer'sdisease(AD).Therefore,itisnecessarytodevelopasensitiveanalyticalmethodforBMAA,anemergingcyanobacterialtoxin,todeterminewhetheratraceamountisdetectedinthewaterresourcesandtreatedwater.Inthisstudy,wedevelopedasimpleandsensitiveanalyticalmethodforBMAAusingliquidchromatography-tandemmassspectrometry(LC-MS/MS)withdirectinjection.Themethodwasvalidatedforlinearityofcalibration,limitofdetection,limitofquantitation,accuracy,andprecision.Thelimitsofdetectionandquantitationwereintherangeof0.030?/Land0.096?/L,respectively.TheoptimizedmethodwasusedtomeasuretheconcentrationsofBMAAinsurfacewaterfromeachweirpointoftheGeumRiver,NakdongRiver.SamplingandanalysisofdrinkingwatertreatmentplantsoftheGeumRiver,NakdongRiverwereappliedtosamplesforeachprocess.
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고분해능 질량분석장치를 이용한 동시분석법 1. 수계의 유기인계 농약-1
최재원 ( Jae Won Choi ),김윤석 ( Yun Seok Kim ) 한국환경분석학회 2010 환경분석과 독성보건 Vol.13 No.4
A gas chromatography-high resolution mass spectrometry (GC-HRMS) method with solid-phase extraction has been developed for the quantitation of organophosphorous pesticides in surface water. Target compounds in this study were bromacil, cyanazine, dichlorovos (DDVP), metribuzin, phorate, propazine, trifluralin, edifenphos, molinate, iprobenfos (kitazine), diazinon, parathion ethyl, fenitrothion, parathion methyl, simazine and chlorpyrifos. Prior to sample analysis, solid-phase extraction was optimized using RP-1, FL-PR, C18, PESTICIDE, ENVI18 and LRC-SI. The result of the recovery test showed there was no ideal SPE cartridge to produce over 80% recovery. The order of recoveries was RP-1>PESTICIDE>C18>ENVI18>FL-PR>LRCSI. The use of a 5% acetone in dichloromethane helped to increase the recovery rates for some pesticides. Method detection limits of HRMS using RP-1 ranged from 2.2 to 11 ng/L for all of target compounds. The method was applied to the measurement of organophosphorus pesticide residues in surface water (n=56) from Han River. Major pesticides detected in the samples were iprobenfos (nd~160 ng/L), chlorpyrifos (nd~10 ng/L) and others with the low ranges of ng/L. Higher concentrations for these compounds were observed in sites close to highly populated or agricultural area. The use of HRMS with optimized SPE provides increasing sensitivity of detection for target compounds.
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