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高效液相色谱法检测水中5种微囊藻毒素

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毛敬英, 杨敏, 狄一安, 曹金玲, 任立军, 许其功, 席北斗. 高效液相色谱法检测水中5种微囊藻毒素[J]. 环境工程学报, 2012, 6(11): 3882-3888.
引用本文: 毛敬英, 杨敏, 狄一安, 曹金玲, 任立军, 许其功, 席北斗. 高效液相色谱法检测水中5种微囊藻毒素[J]. 环境工程学报, 2012, 6(11): 3882-3888.
shu
Mao Jingying, Yang Min, Di Yian, Cao Jinling, Ren Lijun, Xu Qigong, Xi Beidou. Detection of 5 variants microcystins in waters using high performance liquid chromatography[J]. Chinese Journal of Environmental Engineering, 2012, 6(11): 3882-3888.
Citation: Mao Jingying, Yang Min, Di Yian, Cao Jinling, Ren Lijun, Xu Qigong, Xi Beidou. Detection of 5 variants microcystins in waters using high performance liquid chromatography[J]. Chinese Journal of Environmental Engineering, 2012, 6(11): 3882-3888.
shu

高效液相色谱法检测水中5种微囊藻毒素

  • 1.

    西南交通大学地球科学与环境工程学院,成都 610031

  • 2.

    中日环境友好保护中心,北京 100029

  • 3.

    中国环境科学研究院水环境系统工程研究室,北京 100012

  • 4.

    中国环境科学研究院 环境基准与风险评估国家重点实验室,北京 100012

  • 基金项目:

    国家"973"重点基础研究发展规划项目(2008CB418006)

    国家"水体污染控制与治理"科技重大专项(2009ZX07106-001)

  • 中图分类号: X832

Detection of 5 variants microcystins in waters using high performance liquid chromatography

  • 1.

    School of Earth Science and Environmental Engineering, Southwest Jiaotong University, Chengdu 610031, China

  • 2.

    Sino-Japanese Friendship Environment Protection Center,Beijing 100029

  • 3.

    Laboratory of Water Environmental System Engineering, Chinese Research Academy of Environmental Sciences, Beijing 100012, China

  • 4.

    State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China

  • Fund Project:

  • 摘要: 使用Agilent1260型高效液相色谱仪,建立定量测定天然水体中5种微囊藻毒素(MC-RR、YR、LR、LA、LY)的分析方法。比较甲醇/三氟乙酸(TFA)水溶液与甲醇/磷酸两种流动相体系,待测物质的响应程度,结果发现,TFA作为缓冲溶液时,基线较磷酸稳定,因此,选择甲醇/TFA水溶液作为流动相。比较不同TFA体积比例,待测物质的分离程度,结果显示,甲醇/0.02%的TFA水溶液作为流动相时,5种MCs含量的分离度较好。比较等度和梯度洗脱条件,发现,梯度洗脱条件5种MCs的分离度较等度洗脱条件好。该方法MC-RR、YR、LR、LA、LY 的最低检出限(LOD)分别为0.015、0.035、0.018、0.032和0.026 μg/L,最低定量限(LOQ)分别是0.049、0.117、0.062、0.106和0.086 μg/L。在0.10~1.50 μg/mL 的线性范围内,相关系数R2≥0.99,实际水样回收率为73.9%~103.3%。
    Abstract: A method using high performance liquid chromatography (HPLC) was described for the determination of trace amount of microcystins (MCs), MC-RR, MC-YR, MC-LR, MC-LA and MC-LY) in natural waters. The responses of MCs using two different mobile phases, methanol/trifluoroacetic acid aqueous and methanol/phosphate, were compared. The result showed that the base line was more stable using trifluoroethanoic acid as the buffer solution than phosphate. Furthermore, different ratios of trifluoroethanoic acid were used as water phase, the results indicated that best separation was obtained using 0.02% trifluoroethanoic acid as mobile phase. In addition, five kinds of MCs were separated in 12 min under the condition of gradient mobile phase (methanol/water with 0.02%). The limits of detection (LOD) of this method were 0.015, 0.035, 0.018, 0.032, 0.026 μg/L and the limits of quantification (LOQs) were 0.049, 0.117 0.062, 0.106, 0.086 μg/L for MC-RR, MC-YR, MC-LR MC-LA, MC-LY, respectively. The correlation coefficients were ≥0.99 between 0.10~1.50 μg/mL, recoveries of the five variants were in the range of 73.9%~103.3%.
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  • [1] 张敬平,肖付刚,赵晓联,等.微囊藻毒素分析检测技术.北京:化学工业出版社,2009:29-32
    [2] 郁晞,高红梅,彭丽霞,等.淀山湖微囊藻毒素-LR的污染状况及居民肝功能的调查.环境与职业医学,2010,27(3):153-155 Yu Xi, Gao Hongmei, Peng Lixia, et al,Study on pollution level of microcystin in lake water and liver function of local residents around dianshan lake. Environ. Occup. Med.,2010,27 (3): 153-155(in Chinese)
    [3] 穆丽娜,陈传炜,俞顺章,等.太湖水体微藻毒素含量调查及其处理方法研究.中国公共卫生,2000,16(9):803-804 Mu Lina,Chen Chuanwei,Yu Shunzhang, et al. Investigation study on the content of microcystion in tai lake and methods for microcystion treatment. China Public Health, 2000,16(9):803-804(in Chinese)
    [4] 潘晓洁,常锋毅,沈银武,等.滇池水体中微囊藻毒素含量变化与环境因子的相关性研究.湖泊科学.2006,18(6):572-578 Pan Xiaojie,Chang Fengyi,Shen Yinwu,et al.The correlation between the variation of microcystin content and environment factors in Dianchi Lake.Lake Sci.,2006,18(6):572-578(in Chinese)
    [5] 郑利,谢平,林匡飞,等.武汉莲花湖微囊藻毒素含量的变化特征及其影响因素的研究.农业环境科学学报,2004,23(6):1053-1057 Zheng Li,Xie Ping,Lin Kuangfei,et al.Variation characteristics of microcystin concentration and influencing factors in Lianhua Lake (Wuhan).Journal of Agro-Environment Science,2004,23(6):1053-1057(in Chinese)
    [6] 施玮,吴和岩,赵耐青,等.淀山湖水质富营养化和微囊藻毒素污染水平.环境科学2005,26(5):55-61 Shi Wei, Wu Heyan, Zhao Naiqing,et al. Eutrophication and pollution level of microcystin in Dianshan Lake. Environmental Science,2005,26(5):55-61(in Chinese)
    [7] 何振荣,俞家禄,何家苑,等.东湖蓝藻水华毒性的研究Ⅱ:季节变化及微囊藻的毒性.水生生物学报1989,13(3):201-208 He Zhenrong,Yu Jialu,He Jiayuan, et al.Study in East Lake toxic algal blooms.Ⅱ.Seasonal variation and the toxicity of Microcystis.Acta Hydrobiologica Sinica,1989,13(3):201-208(in Chinese)
    [8] 王红兵,刘世杰.微囊藻毒素、佛波酯和苯巴比妥钠对细胞间隙通讯和细胞内Ca(2+)浓度的影响.北京医科大学学报,1998,30(6):568-570 Wang Hongbing, Liu Shijie. Effcts of microcystins, phenobarbital sodium and tetradecanoylphorbol acetate on gap-junction intercellular communiation and intracellular free Ca2 + in BALB/c3T3 cells. Journal of Beijing Medical Univercity,1998,30(6):568-570(in Chinese)
    [9] 董传辉,俞顺章,陈刚,等.江苏几个地区与某湖周围水厂不同型水微囊藻毒素调查.环境与健康杂志,1998,15(3).111-113 Dong Chuanhui,Yu Shunzhang, Chen Gang, et al. Detection of microcystins in water samples came from four zones and a lake of Jiangsu Province.Journal of Environment and Health, 1998,15(3).111-113(in Chinese)
    [10] 孟玉珍,张丁,王兴国等.郑州市水源水藻类和藻类毒素污染调查卫生研究,1999,28(2):100-101 MengYuzhen, Zhang Ding, Wang Xingguo. et al. Study on the contamination of algae and microcystins in water sources of Zhengzhou City. Journal of Hygiene Research, 1999,28(2):100-101(in Chinese)
    [11] 孙昌盛,陈华,薛常镐,等.同安水环境藻类及藻类毒素分布调查.中国公共卫生,2000,16(2):147-148 Sun Changsheng,Chen Huan,Xue Changgao. et al. Study of distribution of algal toxin and algal species in Tongan environment. China Public Health. 2000,16(2):147-148(in Chinese)
    [12] 殷娣娣,高乃云,黎雷.水体微囊藻毒素表征指标检测方法综述.上海环境科学,2010,29(5):213-230 Yin Didi, Gao Naiyun, Li Lei. A review on methods for the determination of conventional indicators for microcystin in eutrophic waters. Shanghai Environmental Sciences, 2010,29(5):213-230(in Chinese)
    [13] 刘碧波,肖邦定,刘剑彤,等.天然水体中痕量微囊藻毒素的高效液相色谱测定方法优化.分析化学,2005,33(11):1577-1579 Liu Bibo, Xiao Bangding, Liu Jiantong,et al. The Optimization of high performance liquid chromatographic method for analysis of trace microcystin s in natural water bodies. Chinese Journal of Analytical Chemistry,2005,33(11):1577-1579(in Chinese)
    [14] 张维昊,方涛,徐小清,等.滇池水华蓝藻中微囊藻毒素的光降解研究.中国环境科学,2001,21:19-22 Zhang Weihao,Fang Tao,Xu Xiaoqing, et al. Study on photodegradation of cyanobacterial toxin in blooms of Dianchi Lake.China Environmental Science, 2001,21:19-22(in Chinese)
    [15] 肖付刚,赵晓联,汤坚,等. 免疫亲和层析-液质联用法检测蓝藻中的微囊藻毒素.分析化学,2009,37(3):369-372 Xiao Fugang,Zhao Xiaolian,Tang Jian,et al. Determination of microcystins in cyanobacteria using immunoaffinity chromatography column and high performance liquid chromatography/mass spectrometry.Chinese Journal of Analytical Chemistry,2009,37(3):369-372(in Chinese)
    [16] 虞锐鹏,陶冠军,秦方,等.液相色谱-电喷雾电离质谱法测定水中的微囊藻毒素.分析化学,2003,31(12):1462-1464 Yu Ruipeng, Tao Guanjun, Qing Fang, et al. Identification and quantification of microcystins in water by high performance liquid chromatography-electrospray ionization mass spectrometry. Chinese Journal of Analytical Chemistry, 2003,31(12):1462-1464(in Chinese)
    [17] Chunlin Ge, Fengming Luan, Ning Ma, et al. Diagnosis of tumor-like polypoid lesions of gallbladder by serumproteomic fingerprint foxicon. Chinese Journal of Cancer Research, 2008,20(4):286-289
    [18] Ruangyuttikarn.W.,Miksik.I.,et al.Reversed-phaseliquidchromatographic-mass spectrometric determination of microcystin-LR in cyanobacteria blooms under alkaline conditions.Chromatogr.B,2004,800(122):315-319
    [19] Dai.M.,Xie.P.,LiangG.D.,et al.Simultaneous determination of microcystin-LR and its glutathione conjugate in fish tissues by liquid chromatography-tandem mass spectrometry.Chromatogr.B,2008,862(122):43-50
    [20] 聂晶晶,李元,李琴,等.微囊藻毒素检测方法的研究进展.中国环境监测,2007,23(2):43-48 Nie Jingjing,Li Yuan.,Li Qin,et al.Progress on techniques of determining microcystins. Environmental Monitoring in China, 2007,23(2):43-48(in Chinese)
    [21] 中华人民共和国卫生部.GB5749-2006 生活饮用水卫生规范.北京,2006
    [22] 顾志伟,邵国健,余娟,等,水中微囊藻毒素检测技术进展. 浙江预防医学,2011,23(3):24-27 Gu Zhiwei,Shao Guojian,Yu Juan,et al.Development in microcystins analysis in natural water. Zhejiang Preventive Medicine, 2011,23(3):24-27(in Chinese)
    [23] 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.分析化学,2010,38(5):740-742 Liang Lili,Gong Aijun,Li Hongmei,et al. Determination of microcystins in aquatic environment with high performance liquid chromatography. Chinese Journal of Analytical Chemistry,2010,38(5):740-742(in Chinese)
    [24] 沈红娜,周建威,袁帅.高效液相色谱法测定喀斯特型高原深水水库中的微囊藻毒素的含量.贵州师范大学学报(自然科学版),2011,29(1):95-98 Shen Hongna,Zhou Jianwei,Yuan Shuai.Determination of microcystin by high performance liquid chromatograph in Aha Lake which is karst-type plateau deep-water reservoir located in Guizhou. Journal of Guizhou Normal University(Natural Sciences),2011,29(1):95-98(in Chinese)
    [25] 张立将,尹立红,浦跃朴,等.水中微囊藻毒素高效液相色谱检测与前处理条件优化.东南大学学报(自然科学版),2005,35(3):446-451 Zhang Lijiang,Yin Lihong,Pu Yuepu,et al.Optimization in analysis and sample preparation of microcystinsin water with high-performance liquid chromatography. Journal of Southeast University (Natural Science Edition),2005,35(3):446-451(in Chinese)
    [26] Ikawa M., Phillips N.,Haney J.F.,et al.Interference by plastics additives in the HPLC determination of microcystin-LR and-YR.Toxicon,1999,37(6):923-929
    [27] 邵国健,吴丹青,余娟.固相萃取HPLC法测定太湖水中3种微囊藻毒素.中国卫生检验杂志,2011,21(1)72-75 Shao Guojian, Wu Danqing, Yu Juan. Determination of three microcystins in Tai Lake by solid phase extraction-high performance liquid chromatography. Chinese Journal of Health Laboratory Technology, 2011,21(1)72-75(in Chinese)
    [28] 戚莉莉,程子波,邹华,等.高效液相色谱法测定太湖水中微囊藻毒素.食品与生物技术报,2009,28(1):97-101 Qi Lili, Chen Zibo,Zou Hua,et al. HPLC Determination of microcystin in Tai Lake. Journal of Food Science and Biotechnology, 2009,28(1):97-101(in Chinese)
    [29] 王金丽,梁文艳,陈莉.微囊藻毒素MC-LR的分离与纯化.北京林业大学学报.2010,32(2):184-188 Wang Jinli,Liang Wenyan,Chen Li.Separation and purification of microcystin-LR. Journal of Beijing Forestry University,2010,32(2) 184-188(in Chinese)
    [30] 张维昊,肖邦定,方涛,等.天然水华蓝藻中微囊藻毒素的提取和净化研究.环境污染与防治,2004,25(5):265-267 Zhang Weihao,Xiao Bangding,Fang Tao,et al.Extraction and purification of microcystins from natural cyanobacterial bloom. Environmental Pollution Prevention,2004,25(5):265-267(in Chinese)
    [31] 国家环境保护总局.HJ/T168-2010 环境监测分析方法标准制订技术导则.北京,2010
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  • 收稿日期:  2011-12-22
  • 刊出日期:  2012-11-09
毛敬英, 杨敏, 狄一安, 曹金玲, 任立军, 许其功, 席北斗. 高效液相色谱法检测水中5种微囊藻毒素[J]. 环境工程学报, 2012, 6(11): 3882-3888.
引用本文: 毛敬英, 杨敏, 狄一安, 曹金玲, 任立军, 许其功, 席北斗. 高效液相色谱法检测水中5种微囊藻毒素[J]. 环境工程学报, 2012, 6(11): 3882-3888.
shu
Mao Jingying, Yang Min, Di Yian, Cao Jinling, Ren Lijun, Xu Qigong, Xi Beidou. Detection of 5 variants microcystins in waters using high performance liquid chromatography[J]. Chinese Journal of Environmental Engineering, 2012, 6(11): 3882-3888.
Citation: Mao Jingying, Yang Min, Di Yian, Cao Jinling, Ren Lijun, Xu Qigong, Xi Beidou. Detection of 5 variants microcystins in waters using high performance liquid chromatography[J]. Chinese Journal of Environmental Engineering, 2012, 6(11): 3882-3888.
shu

高效液相色谱法检测水中5种微囊藻毒素

  • 1.  西南交通大学地球科学与环境工程学院,成都 610031
  • 2.  中日环境友好保护中心,北京 100029
  • 3.  中国环境科学研究院水环境系统工程研究室,北京 100012
  • 4.  中国环境科学研究院 环境基准与风险评估国家重点实验室,北京 100012
  • 收稿日期:  2011-12-22
基金项目:

国家"973"重点基础研究发展规划项目(2008CB418006)

国家"水体污染控制与治理"科技重大专项(2009ZX07106-001)

摘要: 使用Agilent1260型高效液相色谱仪,建立定量测定天然水体中5种微囊藻毒素(MC-RR、YR、LR、LA、LY)的分析方法。比较甲醇/三氟乙酸(TFA)水溶液与甲醇/磷酸两种流动相体系,待测物质的响应程度,结果发现,TFA作为缓冲溶液时,基线较磷酸稳定,因此,选择甲醇/TFA水溶液作为流动相。比较不同TFA体积比例,待测物质的分离程度,结果显示,甲醇/0.02%的TFA水溶液作为流动相时,5种MCs含量的分离度较好。比较等度和梯度洗脱条件,发现,梯度洗脱条件5种MCs的分离度较等度洗脱条件好。该方法MC-RR、YR、LR、LA、LY 的最低检出限(LOD)分别为0.015、0.035、0.018、0.032和0.026 μg/L,最低定量限(LOQ)分别是0.049、0.117、0.062、0.106和0.086 μg/L。在0.10~1.50 μg/mL 的线性范围内,相关系数R2≥0.99,实际水样回收率为73.9%~103.3%。

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