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30 7 2011 7 ENVIRONMENTAL CHEMISTRY Vol 30No 7 July 2011 - N- * NDMA ** 100124 - GC-MS N- NDMA SPE SPE NDMA activated coconut charcoal SPE NDMA 1 μg L - 1 5 ng L - 1 15 μg L - 1 100 μg L - 1 NDMA 88 5% 100 8% SPE ph ph 2 5 9 8 NDMA SPE 5 N- - N- NNC N- NDMA NCC 1-3 NDMA 4-5 NDMA 6 2007 US EPA NDMA 7 ng L - 13 NDMA 7-9 NDMA 10-12 SPE 2004 USEPA 13 Lichrolut EN Ambersorb 572 RDL1 6 ng L - 1 Stephen 14 Carboxen 564 15 SPE /LC /MS /MS NDMA 81% 108% SPE - - GC-MS SPE NDMA SPE-GC-MS NDMA 1 1 1 - GC-MS Thermo Fisher Scientific DSQEI Agilent J&W DB-170130 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 99 999% BIP Technologies Experis Gases Milli-Q NDMA100 ng μl - 1 Dr Ehrenstorfer GmbH 2010 8 12 * 20903006 2008B09 2092008 2010467032 ** Tel010-67391667E-mailydliu@ bjut edu cn

1328 30 1 2 SPE SPE 5 ml 600 mg activated coconut charcoal 20 40 1070 m 2 g - 1 NDMA SPE 1 min2 3 ml min - 1 2 ml 0 25 μm 1 3 GC-MS 45 5 min 10 min - 1 200 5 min 200 1 0 ml min - 1 230 250 3 50 minfull Scan 25 100SIM 74 42 28 1 μlei 70 ev 1 4 100 ng μl - 1 NDMA 1 ml 100 ml 0 1 mol L - 1 NaNO 2 0 1 mol L - 1 NaOH 0 1 mol L - 1 NaH 2 PO 4 0 1 mol L - 1 Na 2 HPO 4 NDMA 10 ml NDMA 15 μg L - 1 100 μg L - 1 GC-MS NDMA NDMA 1 5 1 mg L - 1 0 5 mg L - 1 0 25 mg L - 1 0 1mg L - 1 0 05 mg L - 1 N- NDMA Y = 2000000X + 21004 R 2 = 0 9983 Y 74 NDMA SIM X NDMA mg L - 1 3 S /N NDMA 1 μg L - 1 2 2 1 SPE 5 SPE Agela-PCX Agela-C18 Agela-PEP C 1 SPE Sepulco C 2 SPE Agela-PCX SPE / 35 μm 80 600 m 2 g - 1 Agela-C18SPE C18 45 μm 60 480 m 2 g - 1 Agela-PEP SPE / 35 μm 80 600 m 2 g - 1 C 1 SPE 30 50 800 1100 m 2 g - 1 Sepulco activated coconut charcoalc 2 SPE 20 40 1070 m 2 g - 1 5 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 - 1 10 ml 1 2 2 ml 1 μl GC-MS 3 5 SPE NDMA 1

7 - N- NDMA 1329 1 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 1 1 5 SPE NDMA The adsorbtion of NDMA on five different SPE columns SPE /% 100 μg L - 1 RSD /% n = 3 PCX - - C18 39 1 23 1 PEP 45 6 19 4 C 1 69 1 5 6 C 2 98 6 2 7 2 2 2 ml GC-MS NDMA NDMA 1 2 1 ml 2 ml 3 ml 4 ml 5 ml 10 ml 100 μg L - 1 NDMA 2 ml 3 0 1 mol L - 1 NaNO 2 0 1 mol L - 1 NaOH 0 1 mol L - 1 NaH 2 PO 4 0 1 mol L - 1 Na 2 HPO 4 1 5 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 3 2 2 NDMA 15 μg L - 1 100 μg L - 1 NDMA 88 5% 100 8% NDMA

1330 30 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 = 3 15 100 13 27 88 5 3 04 14 1 94 4 23 98 6 98 6 2 40 101 100 8 3 21 2 4 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 2 5 9 8 SPE NDMA 77 3% 99 1% ph 2 8 6 3 77 3% 90 4% ph 2 6 ph 3 4 5 6 ph 6 3 9 8 91 7% 99 1% NDMA SPE 2 5 SPE SPE 3 6 5 92 4% 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 = 6 4 90 5 mmol L - 1 5 mmol L - 1 4 h NDMA 0 45 mg L - 1 3 SPE-GC-MS NDMA 88 5% 100 8%

7 - N- NDMA 1331 MDL = 5 ng L - 1 ph 2 5 9 8 5 NDMA NDMA 1Bogovski PBogovski S Special report animal species in which N-nitroso compounds induce cancer J Int J Cancer198127 4 471-474 2 N- M 1988196 3U S Environmental Protection Agency USEPA Integrated Risk Information SystemIRIS Office of Research and Development ORD OL 2010-05-15 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 Sci200320 5 389-404 5Charrois JArend MFroese Ket al Detecting N-nitrosamines in drinking water at nanogram per liter levels using ammonia positive chemical ionization J Environ Sci Technol200438 184835-4841 6Mitch WSedlak D Formation of N-nitrosodimethylamine NDMAfrom dimethylamine during chlorination J Environ Sci Technol 200236 4 588-595 7Sun ZLiu YZhong R Theoreticalinvestigation of N-nitrosodimethylamine formation from nitrosation of trimethylamine J J Phys Chem A2010114 1 455-465 8Schreiber IMitch W Influence of the order of reagent addition on NDMA formation during chloramination J Environ Sci Technol 200539 103811-3818 9 NDMA J 2008 29 7 1908-1913 10Schreiber IMitch W Nitrosamine formation pathway revisitedthe importance of chloramine speciation and dissolved oxygen J Environ Sci Technol200640 196007-6014 11Andrzejewski PKasprzyk-Hordern BNawrocki J The hazard of N-nitrosodimethylamineNDMAformation during water disinfection with strong oxidants J Desalination2005176 1-3 37-45 12 N- M 198050-59 13Method 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 /0542005 14Stephen WCarolyn JVincent Yet al N-nitrosodimethylamine in drinking water using a rapidsolid-phase extraction method J ESPR-Environ Sci & Pollut Res19952 4 207-210 15 SPE /LC /MS /MS J 2009 25 1482-92 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 2 5 9 8 In addition the SPE column could be reused for up to five times KeywordsN-nitrosodimethylamine GC-MS SPE