ENVIRONMENTAL CHEMISTRY

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1 ENVIRONMENTAL CHEMISTRY Vol 30No 7 July N- * NDMA ** GC-MS N- NDMA SPE SPE NDMA activated coconut charcoal SPE NDMA 1 μg L ng L μg L μg L - 1 NDMA 88 5% 100 8% SPE ph ph NDMA SPE 5 N- - N- NNC N- NDMA NCC 1-3 NDMA 4-5 NDMA US EPA NDMA 7 ng L - 13 NDMA 7-9 NDMA SPE 2004 USEPA 13 Lichrolut EN Ambersorb 572 RDL1 6 ng L - 1 Stephen 14 Carboxen SPE /LC /MS /MS NDMA 81% 108% SPE - - GC-MS SPE NDMA SPE-GC-MS NDMA GC-MS Thermo Fisher Scientific DSQEI Agilent J&W DB m 0 25 mm 0 25 μm Agela-PCX Agela-C18 Agela-PEP Agela Technologies C 1 Agela Technologies C 2 Sepulco 0 10 μl SGE % BIP Technologies Experis Gases Milli-Q NDMA100 ng μl - 1 Dr Ehrenstorfer GmbH * B ** Tel ydliu@ bjut edu cn

2 SPE SPE 5 ml 600 mg activated coconut charcoal m 2 g - 1 NDMA SPE 1 min2 3 ml min ml 0 25 μm 1 3 GC-MS 45 5 min 10 min min ml min minfull Scan SIM μlei 70 ev ng μl - 1 NDMA 1 ml 100 ml 0 1 mol L - 1 NaNO mol L - 1 NaOH 0 1 mol L - 1 NaH 2 PO mol L - 1 Na 2 HPO 4 NDMA 10 ml NDMA 15 μg L μg L - 1 GC-MS NDMA NDMA mg L mg L mg L mg L mg L - 1 N- NDMA Y = X R 2 = Y 74 NDMA SIM X NDMA mg L S /N NDMA 1 μg L SPE 5 SPE Agela-PCX Agela-C18 Agela-PEP C 1 SPE Sepulco C 2 SPE Agela-PCX SPE / 35 μm m 2 g - 1 Agela-C18SPE C18 45 μm m 2 g - 1 Agela-PEP SPE / 35 μm m 2 g - 1 C 1 SPE m 2 g - 1 Sepulco activated coconut charcoalc 2 SPE m 2 g SPE NDMA Agela-PCX 0 1 mol L - 1 NDMA ph 4 1% 1% 3 ml 2 ml 3 SPE 1 2 NDMA 100 μg L ml ml 1 μl GC-MS 3 5 SPE NDMA 1

3 7 - N- NDMA PCX NDMA C18 PEP C 1 NDMA 39 1% 45 6% 69 1% 23 1% 19 4% 5 6% SPE C 2 NDMA 98 6% 2 7% C 2 Table SPE NDMA The adsorbtion of NDMA on five different SPE columns SPE /% 100 μg L - 1 RSD /% n = 3 PCX - - C PEP C C ml GC-MS NDMA NDMA ml 2 ml 3 ml 4 ml 5 ml 10 ml 100 μg L - 1 NDMA 2 ml mol L - 1 NaNO mol L - 1 NaOH 0 1 mol L - 1 NaH 2 PO mol L - 1 Na 2 HPO ml NDMA 86 2% 97 5% 5 ml NDMA GC-MS 1 ml 2 ml TIC NDMA 3 ml TIC 4 ml 4 ml NDMA 3 ml Fig 1 1 NDMA The recovery efficiency of NDMA with different leaching liquid volumes 2 3 NDMA SPE 2 NDMA SPE 10 ml 2 ml1 μl GC-MS NDMA 15 μg L μg L - 1 NDMA 88 5% 100 8% NDMA

4 NDMA Table 2 2 NDMA The recovery efficiency of NDMA with different water solution matrixes NDMA /μg L - 1 NDMA /μg L - 1 /% RSD /% n = SPE SPE ph NDMA 0 5 mg L - 1 ph 0 1 mol L - 1 NaOH 0 1 mol L - 1 HCl 0 5 mg L - 1 NDMA 3 2 ph SPE NDMA 77 3% 99 1% ph % 90 4% ph 2 6 ph ph % 99 1% NDMA SPE 2 5 SPE SPE % 105% SPE NDMA SPE NDMA 2 Fig 2 ph NDMA The recovery efficiency of NDMA at different ph values 3 NDMA Fig 3 The recovery efficiency of NDMA after repeated column use 2 6 NDMA 1 μg L - 1 MDL5 ng L - 1 SPE-GC-MS 200 NDMA NDMA ph = mmol L mmol L h NDMA 0 45 mg L SPE-GC-MS NDMA 88 5% 100 8%

5 7 - N- NDMA 1331 MDL = 5 ng L - 1 ph NDMA NDMA 1Bogovski PBogovski S Special report animal species in which N-nitroso compounds induce cancer J Int J Cancer N- M U S Environmental Protection Agency USEPA Integrated Risk Information SystemIRIS Office of Research and Development ORD OL http/ /www epa gov /iris /subst /0045 htm 4Mitch WSharp JTrussell RValentine Ret al N-nitrosodimethylamine NDMAas a drinking water contaminanta review J Environ Eng Sci Charrois JArend MFroese Ket al Detecting N-nitrosamines in drinking water at nanogram per liter levels using ammonia positive chemical ionization J Environ Sci Technol Mitch WSedlak D Formation of N-nitrosodimethylamine NDMAfrom dimethylamine during chlorination J Environ Sci Technol Sun ZLiu YZhong R Theoreticalinvestigation of N-nitrosodimethylamine formation from nitrosation of trimethylamine J J Phys Chem A Schreiber IMitch W Influence of the order of reagent addition on NDMA formation during chloramination J Environ Sci Technol NDMA J Schreiber IMitch W Nitrosamine formation pathway revisitedthe importance of chloramine speciation and dissolved oxygen J Environ Sci Technol Andrzejewski PKasprzyk-Hordern BNawrocki J The hazard of N-nitrosodimethylamineNDMAformation during water disinfection with strong oxidants J Desalination N- M Method 521Determination of nitrosamines in drinking water by solid phase extraction and capillary column gas chromatography with large volume injection and chemical ionization tandem mass spectrometryms /MS S U S Environmental Protection AgencyWashington DCEPA /600 /R-05 / Stephen WCarolyn JVincent Yet al N-nitrosodimethylamine in drinking water using a rapidsolid-phase extraction method J ESPR-Environ Sci & Pollut Res SPE /LC /MS /MS J AN SPE METHOD FOR GC-MS ANALYSIS OF N-NITROSODIMETHYLAMINE IN DRINKING WATER LIU Qingming ZHANG Xuechen ZHOU Quan LIU Yongdong ZHONG Rugang College of Life Science & Bioengineering Beijing University of TechnologyBeijing100124China ABSTRACT In this papera solid-phase extraction SPEmethod suitable for gas chromatography-mass spectrometry GC-MSto detect the N-nitrosodimethylamine NDMAin drinking water was established By comparing SPE columns with different fillingsthe SPE column with the activated coconut charcoal was found to have good selectivity in extraction NDMA from waterwith the instrument and method detection limits being 1 μg L - 1 and 5 ng L - 1 respectively For the two different matrix solutions with NDMA concentrations of 15 μg L - 1 and 100 μg L - 1 respectivelythe average recovery rate was 88 5% 100 8% The SPE method was found to be effective over a wide range of phand the extraction of NDMA was slightly affected in the range of ph In addition the SPE column could be reused for up to five times KeywordsN-nitrosodimethylamine GC-MS SPE

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