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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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  • 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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