DOI: 10.3724/SP.J.1096.2013.30393

Chinese Journal of Analytical Chemistry (分析化学) 2013/41:12 PP.1844-1850

Determination of Five Microcystins in Cyanobacteria by Liquid Chromatography Tandem Mass Spectrometry Using Freezing-thawing and Solid Phase Extraction

A method was developed for simultaneous determination of five microcystins(MCs) in Cyanobacteria by liquid chromatography Tandem mass spectrometry(LC-MS/MS) using freezing-thawing and solid phase extraction(SPE). Cyanobacteria in environmental water was collected by 0.45 μm hybrid filter and extracted with two times of 5 mL 75% methanol after three times of -20℃/37℃ freezing-thawing. The extract was concentrated by end-capped C18 SPE cartridge with a clean-up by 10 mL 5% methanol. Five MCs were detected by LC-MS/MS with multiple reaction monitoring and external standard method. Gradient elution was employed with a mobile phase consisting of acetonitrile with 0.1% formic acid and water with 0.1% formic acid on C18 column (50 mm×2.1 mm, 1.7 μm). The method showed good linear correlations in a range of 1.25-50 μg/L with correlation coefficients greater than 0.995. RSD and LOD were 3.0%-11.5% and 0.05-0.2 ng, respectively. Recovery of three spiked levels (1, 5 and 50 ng) for five MCs were 63.7%-100.4% (RSD 5.5%-13.1%), 72.6%-85.7% (RSD 3.1%-6.6%) and 72.5%-80.5% (RSD 2.6%-8.3%), respectively. The proposed method was applied in the detection of intracellular and extracellular MCs in one drinking water source of South China from August to December.

Key words:Microcystin,Liquid chromatography Tandem mass spectrometry,Cyanobacteria,Freezing-thawing,Solid phase extraction

ReleaseDate:2015-04-19 11:08:01

1 Martin W, Hans D. FEMS Microbiol. Rev., 2006, 30(4): 530-63

李 砚, 舒为群. 环境与健康杂志, 2010, 27(8): 730-733

2 Diehnelt C W, Dugan N R, Peterman S M, Budde W L. Anal. Chem., 2006, 78(2): 501-512

生活饮用水卫生标准. 中华人民共和国国家标准. GB/T 5749-2006

蔡金傍, 李文奇, 逄 勇, 杨旭光. 水利学报, 2009, 40(3): 328-334

3 Ueno Y, Nagata S, Tsutsumi T, Hasegawa A, Watanabe M F, Park H D, Chen G C, Chen G, Yu S Z. Carcinogenesis, 1996, 17(6): 1317-1321

4 LI Yan, SHU Wei-Qun. Journal of Environment and Health, 2010, 27(8): 730-733

郭 坚, 杨新磊, 叶明立. 分析化学, 2011, 39(8): 1256-1260

5 Cogliano V J, Baan R A, Straif K, Grosse Y, Secretan B, Ghissassi F. Environmental and Molecular Mutagenesis, 2008, 49(2): 100-109

王 超, 吕怡兵, 许人骥, 陈 烨, 阴 琨, 滕恩江. 色谱, 2011, 29(3): 212-216

吴伟文, 杨左军, 顾浩飞, 郑文丽, 徐 嵘. 分析测试学报, 2007, 26(4): 545-547

6 World Health Organization(WHO). Guidelines for Drinking-water Quality: Incorporating 1st and 2nd Addenda, Vol.1, Recommendations. 3rd ed. 2008: 195

7 Chorus I, Bartram J. Toxic Cyanobacteria in Water: a Guide to Their Public Health Consequences, Monitoring, Management. Taylor & Francis, 1999: 141

郭 坚, 杨新磊, 叶明立. 分析化学, 2011, 39(8): 1256-1260

8 GB/T 5749-2006, Standards for Drinking Water Quality. National Standards of the People's Republic of China

肖付刚, 赵晓联, 汤 坚, 顾小红, 张敬平, 钮伟民. 分析化学, 2009, 37(3): 369-372

肖付刚, 赵晓联, 汤 坚, 顾小红, 张敬平, 钮伟民. 分析化学, 2008, 36(1): 99-102

9 Figueiredo D R, Azeiteiro U M, Esteves S M, Gonçalves F J M, Pereira M J. Ecotoxicology and Enoironmental safety, 2004, 59(2): 151-163

10 CAI Jin-Bang, LI Wen-Qi, PANG Yong, YANG Xu-Guang. Journal of Hydraulic Engineering, 2009, 40(3): 328-334

彭 亮, 陈 伟, 宋立荣. 水生生物学报, 2011, 35(4): 708-712

11 GUO Jian, YANG Xin-Lei, YE Ming-Li. Chinese J. Anal. Chem., 2011, 39(8): 1256-1260

12 WANG Chao, LV Yi-Bin, XU Ren-Ji, CHEN Ye, YIN Kun, TENG En-Jiang. Chinese Journal of Chromatography, 2011, 29(3): 212-216

13 WU Wei-Wen,YANG Zhuo-Jun, GU Hao-Fei, ZHENG Wen-Li,XU Rong. Journal of Instrumental Analysis, 2007, 26(4): 545-547

14 GUO Jian, YANG Xin-Le, YE Ming-Li. Chinese J. Anal.Chem., 2011, 39(8): 1256-1260

15 XIAO Fu-Gang, ZHAO Xiao-Lian, TANG Jian, GU Xiao-Hong, ZHANG Jing-Ping, NIU Wei-Min. Chinese J. Anal. Chem., 2009, 37(3): 369-372

16 Song W, de la Cruz A A, Rein K, O'Shea K. Environ. Sci. Technol., 2006, 40(12), 3941-3946

17 XIAO Fu-Gang, ZHAO Xiao-Lian, TANG Jian, GU Xiao-Hong, ZHANG Jing-Ping, NIU Wei-Min. Chinese J. Anal. Chem., 2008, 36(1): 99-102

18 PENG Liang, CHEN Wei, SONG Li-Long. Acta Hydrobiologica Sinica, 2011, 35(4): 708-712

19 Rivasseau C, Martins S, Hennion M C. J. Chromatogr. A, 1998, 799(1-2):155-169

20 Maagd P De, Hendriks A J, Seinen W, Sijm D. Water Research, 1999, 33(3): 677-680

21 Lawtonb L A, Riveraa J, Caixacha J. J. Chromatogr. A, 2005, 1074(1-2): 23-30

22 Lehman E M. Water Resources, 2007, 41(4): 795-802