| Nitrosamine Analysis by Semi-automated SPE and Fully Automated GC-MS/MS |
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학술지명 2013 APCE/KSFEA/APIA
저자 최재원,김윤덕,정중목,Hans-J,Huebsc
발표일 2013-11-05
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Conventional nitrosamine analysis needs manual SPE sample preparation and GC-CI/MS/MSmethod based on EPA method 521(2004). In this study, automated system for samplepreparation and GC-MS was optimized. GC-EI-MS/MS measurement was done by TSQ8000 model with TriPlus auto sampler (Thermo Fisher Scientific). Calibration standards wereautomatically prepared by using the advanced TriPlus CTC technique. For SRM (seltectedreaction monitoring) optimization, fully automated SRM was performed for 9 nitrosamines.SRM optimization was done within a day by using automated SRM. In the normal condition,initial instrumental detection limit (IDL) of NDMA was 3 pg. IDL of other nitrosamines were2-3 pg ranges. This indicates the low ng/L range LOQs of treated water samples.On the other hand, various brand carbon cartridges showed drastic recoveries. This wascompared using automated SPE system (GL Science). Actual operation of SPE system wasmodified into three steps, 1) conditioning and loading 2) drying and elution, and 3) furtherconcentration. Spiking test using real treated water was performed by above system. In termsof S/N ratio, method detection limit (MDL) of NDMA was 1.59 ng/L. MDLs of othernitrosamines were between 0.08 and 0.61 ng/L, respectively. After minor modifications, themethod was used for nationwide nitrosamine monitoring. |