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超高效液相色谱-电喷雾串联四极杆质谱结合内标物测定水体中微囊藻毒素

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李宏, 潘纲, 张洪刚. 超高效液相色谱-电喷雾串联四极杆质谱结合内标物测定水体中微囊藻毒素[J]. 环境化学, 2014, 33(12): 2087-2093. doi: 10.7524/j.issn.0254-6108.2014.12.017
引用本文: 李宏, 潘纲, 张洪刚. 超高效液相色谱-电喷雾串联四极杆质谱结合内标物测定水体中微囊藻毒素[J]. 环境化学, 2014, 33(12): 2087-2093. doi: 10.7524/j.issn.0254-6108.2014.12.017
shu
LI Hong, PAN Gang, ZHANG Honggang. Determination of microcystin in water samples by ultra-performance liquid chromatography-mass spectrometry coupled with internal standard[J]. Environmental Chemistry, 2014, 33(12): 2087-2093. doi: 10.7524/j.issn.0254-6108.2014.12.017
Citation: LI Hong, PAN Gang, ZHANG Honggang. Determination of microcystin in water samples by ultra-performance liquid chromatography-mass spectrometry coupled with internal standard[J]. Environmental Chemistry, 2014, 33(12): 2087-2093. doi: 10.7524/j.issn.0254-6108.2014.12.017
shu

超高效液相色谱-电喷雾串联四极杆质谱结合内标物测定水体中微囊藻毒素

  • 1.

    中国科学院生态环境研究中心, 北京, 100085

  • 基金项目:

    中国科学院生态环境研究中心科技创新项目(YSW2013B05)资助.

Determination of microcystin in water samples by ultra-performance liquid chromatography-mass spectrometry coupled with internal standard

  • 1.

    Research Center for Eco-environmental Sciences, Chinese Academy of Sciences, Beijing, 100085, China

  • Fund Project:

  • 摘要: 本文建立了超高效液相色谱-电喷雾串联四极杆质谱(UPLC-MS/MS)测定水体中MC-RR和MC-LR的方法,比较了内标的加入对不同水样富集体积下MCs测定准确度的影响.结果表明,以乙腈和水(均含0.1%甲酸)为流动相时,MC-RR和MC-LR在Acquity UPLC BEH C18色谱分离柱(2.1 mm×100 mm i.d.粒径1.7 μm,孔径130 Å)于4 min内完全分离.经优化质谱参数,选择m/z 519.8>134.3和995.5>134.6分别为MC-RR、MC-LR质谱检测的定量离子对.方法学验证表明,在所设定的色谱、质谱参数条件下,UPLC-MS/MS对MC-RR和MC-LR的检出限分别为2.0 ng·L-1和1.0 ng·L-1,定量限分别为为6.0 ng·L-1和3.0 ng·L-1,回收率分别达98.9%—106.5%和98.4%—101.5%.测定太湖梅梁湾水样时,当水体中MCs浓度达到UPLC-MS/MS方法定量限20倍时,可通过加入内标物亮氨酸脑啡肽,实现快速(不经过水样富集)且准确(相对标准偏差<5.0%)的MC-RR与MC-LR测定.
    Abstract: Preconcentration of water sample is required for the determination of microcystins using liquid chromatography-mass spectrometry method, during which the matrix effects and loss of substrates may influence the accuracy. An ultra performance liquid chromatography electrospray ionization tandem triple quadrupole/mass spectrometry (UPLC-MS/MS) method was developed to determine microcystins (MC-RR and MC-LR) in water samples, and the impact of internal standard on MCs measurement accuracy under different precocentration volumes were assessed. Results show that when acetonitrile and water (both containing 0.1% formic acid) were used as mobile phase, MC-RR and MC-LR were separated in an acquity UPLC BEH C18 column (2.1 mm×100 mm i.d. particle size 1.7 μm, pore size 130 Å) within 4 mins. Product-ion traces at m/z 519.8>134.3 and 995.5>134.6 were set as quantitative ions of MC-RR and MC-LR, respectively. Upon method validation, the limit of detection (LOD) for MC-RR and MC-LR was 2.0 and 1.0 ng·L-1, the limit of quantification (LOQ) was 6.0 and 3.0 ng·L-1, and the recoveries were in the range of 98.9%—106.5% and 98.4%—101.5%, respectively. When the method was applied for determination of MC-RR and MC-LR in water samples of Taihu Lake, rapid (without preconcentration of water samples) and accurate (RSD<5.0%) determination of MCs was achieved when internal standard (leucine enkephalin) was added in the raw water and microcystins levels were above 20-fold of the LOQ.
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  • [1] 程子波,邹华,向丽,等.叶绿素作用下微囊藻毒素LR的光降解[J].环境化学,2009,28(5):683-686
    [2] Song L, Chen W, Peng L, et al. Distribution and bioaccumulation of microcystins in water columns: A systematic investigation into the environmental fate and the risks associated with microcystins in Meiliang Bay, Lake Taihu[J]. Water Research, 2007, 41(13): 2853-2864
    [3] Chen J, Xie P, Li L, et al. First identification of the hepatotoxic microcystins in the serum of a chronically exposed human population together with indication of hepatocellular damage[J]. Toxicological Sciences, 2009, 108(1): 81-89
    [4] Park H, Namikoshi M, Brittain S M, et al. D-Leu(1) microcystin-LR, a new microcystin isolated from waterbloom in a Canadian prairie lake[J]. Toxicon, 2001, 39(6): 855-862
    [5] 郑西强,刘群,陈云峰.活性炭纤维对水中微囊藻毒素的吸附性能[J].环境工程学报,2013,7(10):3802-3806
    [6] 李铮,杜克久,赵兴茹,等.高效液相色谱法测定天然水体中微囊藻毒素方法优化[J].环境化学,2012, 31(4):545-551
    [7] 张明,唐访良,徐建芬,等.固相萃取-高效液相色谱法同时测定地表水中9种微囊藻毒素[J].环境化学,2013,32(6): 1096-1097
    [8] Churchwell M I, Twaddle N C, Meeker L R, et al. Improving LC-MS sensitivity through increases in chromatographic performance: Comparisons of UPLC-ES/MS/MS to HPLC-ES/MS/MS[J]. Journal of Chromatography B, 2005, 825(2): 134-143
    [9] Xu W, Chen Q, Zhang T, et al. Development and application of ultra performance liquid chromatography-electrospray ionization tandem triple quadrupole mass spectrometry for determination of seven microcystins in water samples[J]. Analytica Chimica Acta, 2008, 626(1): 28-36
    [10] 茅海琼,翁燕波,傅晓钦,等.超高效液相色谱-电喷雾串联四级杆质谱法快速分析水中微囊藻毒素LR[J].中国环境监测,2009,25(6):19-22
    [11] Yen H K, Lin T F, Liao P C. Simultaneous detection of nine cyanotoxins in drinking water using dual solid-phase extraction and liquid chromatography-mass spectrometry[J]. Toxicon, 2011, 58(2): 209-218
    [12] Xiao F G, Zhao X L, Tang J, et al. Determination of Microcystin-LR in Water from Lake Tai, China[J]. Bulletin of Environmental Contamination and Toxicology, 2009, 82(2): 230-233
    [13] 梁丽丽,弓爱君,李红梅,等.高效液相色谱法检测水体中微囊藻毒素[J].分析化学,2010,38(5):740-742
    [14] Wang J, Pang X, Ge F, et al. An ultra-performance liquid chromatography-tandem mass spectrometry method for determination of microcystins occurrence in surface water in Zhejiang Province, China[J]. Toxicon, 2007, 49(8): 1120-1128
    [15] 张春燕,赵兴茹,郑学忠.在线固相萃取超高效液相色谱串联质谱法测定水中微囊藻毒素[J].环境化学,2012, 31(10):1663-1664
    [16] Li W, Duan J, Niu C, et al. Determination of microcystin-lr in drinking water using uplc tandem mass spectrometry-matrix effects and measurement[J]. Journal of Chromatographic Science, 2011, 49(9): 665-670
    [17] Tan A, Lévesque I A, Lévesque I M, et al. Analyte and internal standard cross signal contributions and their impact on quantitation in LC-MS based bioanalysis[J]. Journal of Chromatography B, 2011, 879(21): 1954-1960
    [18] Zenkevich I G, Makarov E D. Chromatographic quantitation at losses of analyte during sample preparation: Application of the modified method of double internal standard[J]. Journal of Chromatography A, 2007, 1150(1/2): 117-123
    [19] Oehrle S A, Southwell B, Westrick J. Detection of various freshwater cyanobacterial toxins using ultra-performance liquid chromatography tandem mass spectrometry[J]. Toxicon, 2010, 55(5): 965-972
    [20] 杨叶,乔善磊,陈景衡,等.同位素内标超高效液相色谱-串联质谱法检测大鼠血清中丙烯酰胺和环氧丙酰胺[J].分析化学研究简报,2010,38(10):1487-1491
    [21] 黄玉娟,陈永山,骆永明,等.气相色谱-质谱联用内标法测定土壤中11 种酞酸酯[J].环境化学,2013,32(4):659-665
    [22] Zhang J, Wang Z, Song Z, et al. Bioaccumulation of microcystins in two freshwater gastropods from a cyanobacteria-bloom plateau lake, Lake Dianchi[J]. Environmental Pollution, 2012, 164: 227-234
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  • 收稿日期:  2014-03-18
李宏, 潘纲, 张洪刚. 超高效液相色谱-电喷雾串联四极杆质谱结合内标物测定水体中微囊藻毒素[J]. 环境化学, 2014, 33(12): 2087-2093. doi: 10.7524/j.issn.0254-6108.2014.12.017
引用本文: 李宏, 潘纲, 张洪刚. 超高效液相色谱-电喷雾串联四极杆质谱结合内标物测定水体中微囊藻毒素[J]. 环境化学, 2014, 33(12): 2087-2093. doi: 10.7524/j.issn.0254-6108.2014.12.017
shu
LI Hong, PAN Gang, ZHANG Honggang. Determination of microcystin in water samples by ultra-performance liquid chromatography-mass spectrometry coupled with internal standard[J]. Environmental Chemistry, 2014, 33(12): 2087-2093. doi: 10.7524/j.issn.0254-6108.2014.12.017
Citation: LI Hong, PAN Gang, ZHANG Honggang. Determination of microcystin in water samples by ultra-performance liquid chromatography-mass spectrometry coupled with internal standard[J]. Environmental Chemistry, 2014, 33(12): 2087-2093. doi: 10.7524/j.issn.0254-6108.2014.12.017
shu

超高效液相色谱-电喷雾串联四极杆质谱结合内标物测定水体中微囊藻毒素

  • 1. 中国科学院生态环境研究中心, 北京, 100085
  • 收稿日期:  2014-03-18
基金项目:

中国科学院生态环境研究中心科技创新项目(YSW2013B05)资助.

摘要: 本文建立了超高效液相色谱-电喷雾串联四极杆质谱(UPLC-MS/MS)测定水体中MC-RR和MC-LR的方法,比较了内标的加入对不同水样富集体积下MCs测定准确度的影响.结果表明,以乙腈和水(均含0.1%甲酸)为流动相时,MC-RR和MC-LR在Acquity UPLC BEH C18色谱分离柱(2.1 mm×100 mm i.d.粒径1.7 μm,孔径130 Å)于4 min内完全分离.经优化质谱参数,选择m/z 519.8>134.3和995.5>134.6分别为MC-RR、MC-LR质谱检测的定量离子对.方法学验证表明,在所设定的色谱、质谱参数条件下,UPLC-MS/MS对MC-RR和MC-LR的检出限分别为2.0 ng·L-1和1.0 ng·L-1,定量限分别为为6.0 ng·L-1和3.0 ng·L-1,回收率分别达98.9%—106.5%和98.4%—101.5%.测定太湖梅梁湾水样时,当水体中MCs浓度达到UPLC-MS/MS方法定量限20倍时,可通过加入内标物亮氨酸脑啡肽,实现快速(不经过水样富集)且准确(相对标准偏差<5.0%)的MC-RR与MC-LR测定.

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