超高效液相色谱-串联质谱法同时测定田螺中3种微囊藻毒素
Simultaneous UHPLC-MS/MS Determination of 3 Microcystic Algae Toxins in Field Snail
摘 要
采用超高效液相色谱-串联质谱法同时测定田螺中3种微囊藻毒素(微囊藻毒素-RR、微囊藻毒素-LR、微囊藻毒素-YR)的含量。田螺样品经甲醇-水(85+15)混合液提取,Oasis HLB固相萃取柱净化。以UPLC BEH C18色谱柱为固定相,以不同体积比混合的(A)甲酸(0.1+99.9)溶液和(B)甲醇-乙腈(1+1)混合液为流动相做梯度洗脱,采用电喷雾正离子源模式多反应监测检测。3种微囊藻毒素的质量浓度均在1.0~100.0 μg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.05~0.08 μg·kg-1之间。以空白样品为基体进行加标回收试验,所得回收率在67.3%~84.2%之间,相对标准偏差(n=6)在6.1%~8.3%之间。
田螺
微囊藻毒素
UHPLC-MS/MS
Field snail
Microcystic algae toxins
Abstract
UHPLC-MS/MS was applied to the simultaneous determination of 3 microcystic algae toxins (MC-RR, MC-LR and MC-YR ) in field snail. The field snail sample was extracted with methanol (85+15) solution and purified by passing through Oasis HLB-solid phase extraction column. UPLC BEH C18 column was used as stationary phase, and mixtures of (A) formic acid (0.1+99.9) aq. solution and (B) mixture of methanol-acetonitrile (1+1) solution mixed in different ratios were used as mobile phase in gradient elution. ESI+ as well as multi-reactions monitoring was adopted in MS/MS. Linear relationships between values of peak area and mass concentration of the 3 microcystic algae toxins were kept in the same range of 1.0-100.0 μg·L-1, with detection limits (3S/N) in the range of 0.05-0.08 μg·kg-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 67.3%-84.2%, with RSD′s (n=6) in the range of 6.1%-8.3%.
中图分类号 O657.63
所属栏目 工作简报
基金项目 国家质检总局科技计划项目(2010QK326)
收稿日期 2013/3/29
修改稿日期
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备注沈坚(1966-)男,浙江宁波人,高级工程师,主要从事食品安全检测技术。
引用该论文: SHEN Jian,ZHANG Ai-zhi,CAO Li-li,WANG Quan-lin. Simultaneous UHPLC-MS/MS Determination of 3 Microcystic Algae Toxins in Field Snail[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(5): 606～610
沈坚,张爱芝,曹丽丽,王全林. 超高效液相色谱-串联质谱法同时测定田螺中3种微囊藻毒素[J]. 理化检验－化学分册, 2014, 50(5): 606～610
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参考文献
【1】区晖,周志洪,吴清柱.高效液相色谱法测定地表水中的微囊藻毒素-LR［J］.广州化学, 2009,34(1):50-53.
【2】UENO Y, NAGATA S, TSUTSUMI T, et al. Detection of microcystins, a blue-green algal hepatotoxin, in drinking water sampled in Haimen and Fusui, endemic area of primary liver cancer in China, by highly sensitive immunoassay［J］. Carcinogenesis, 1996,17(6):1317-1321.
【3】周学富,董传辉,俞顺章.泰安地区肝癌高发因素研究［J］.现代预防医学, 1999(3):350-351.
【4】俞顺章,赵宁,资晓林,等.饮水中微囊藻毒素与我国原发性肝癌关系的研究［J］.中国肿瘤杂志, 2001(23):96-99.
【5】SIVONEN K, JONES G. Cyanobacterial toxins. Chapter 3. In: Chorus I, Bsrtram Jeds. Toxic cyanobacterial in water, a guid to their public health consequences, monitoring and management［M］. London and New York: E & FN Spon, 1999:41-111.
【6】闫建秀.水产品中微囊藻毒素的高效液相色谱检测方法的研究［D］.无锡:江南大学, 2009.
【7】谷康定,林群馨.原代肝细胞和传代细胞对微囊藻毒素-LR的敏感性［J］.毒理学杂志, 2005,19(3):172-174.
【8】BACKER L C, CARMICHAEL W, KIRKPATRICK B, et al. Recreational exposure to low concentrations of microcystins during an algal bloom in a small lake［J］. Marine Drugs, 2008,6(2):389-406.
【9】虞锐鹏,陶冠军,贡小清,等.高效液相色谱-质谱联用方法测定背角无齿蚌体内微囊藻毒素［J］.分析测试学报, 2007,26(5):671-674.
【10】BARCO M, FLORES C, JOSEP R, et al. Determination of microcystin variants and related peptides present in a water bloom of Plank tothrix (oscillatoria) rubescens in a spanish drinking water reservoir by LC/ESI-MS［J］. Toxicon, 2004,44(8):881-886.
【11】周伟杰,刘萍,李雪,等.太湖淡水螺体内微囊藻毒素污染动态研究［J］.实用预防医学, 2012,19(3):349-351.
【12】HARADA K I, MATSUURA K, SUZUKI M, et al. Isolation and characterization of the minor components associated with microcystins LR and RR in the cyanobacterium (blue-green algae)［J］. Toxicon, 1990,28(1):55-64.
【13】刘飞,王勇为.高效液相色谱-串联质谱法测定鲫鱼中的微囊藻毒素［J］.环境化学, 2010,29(4):785-786.
【14】YANG Bo, XU Jin-zhong, DING Tao, et al. A novel method to detect seven microcystins in hard clam and corbicula fluminea by liquid chromatography-tandem mass spectrometry［J］. Journal of Chromatography B, 2009,877(29):3522-3528.
【15】OTT J L, CARMICHAEL W W. LC/ESI/MS method development for the analysis of hepatotoxic cyclic peptide microcystins in animal tissues［J］. Toxicon, 2006,47(7):734-741.
【16】闫建秀,虞锐鹏,汤坚,等.固相萃取-反相高效液相色谱法检测太湖蛳螺中微囊藻毒素［J］.安全与检测, 2008,24(5):92-95.
【17】DAI Ming, XIE Ping, LIANG Gao-dao, et al. Simultaneous determination of microcystin-LR and its glutathione conjugate in fish tissues by liquid chromatography-tandem mass spectrometry［J］. Journal of chromatography B, 2008,862(12):43-50.
【2】UENO Y, NAGATA S, TSUTSUMI T, et al. Detection of microcystins, a blue-green algal hepatotoxin, in drinking water sampled in Haimen and Fusui, endemic area of primary liver cancer in China, by highly sensitive immunoassay［J］. Carcinogenesis, 1996,17(6):1317-1321.
【3】周学富,董传辉,俞顺章.泰安地区肝癌高发因素研究［J］.现代预防医学, 1999(3):350-351.
【4】俞顺章,赵宁,资晓林,等.饮水中微囊藻毒素与我国原发性肝癌关系的研究［J］.中国肿瘤杂志, 2001(23):96-99.
【5】SIVONEN K, JONES G. Cyanobacterial toxins. Chapter 3. In: Chorus I, Bsrtram Jeds. Toxic cyanobacterial in water, a guid to their public health consequences, monitoring and management［M］. London and New York: E & FN Spon, 1999:41-111.
【6】闫建秀.水产品中微囊藻毒素的高效液相色谱检测方法的研究［D］.无锡:江南大学, 2009.
【7】谷康定,林群馨.原代肝细胞和传代细胞对微囊藻毒素-LR的敏感性［J］.毒理学杂志, 2005,19(3):172-174.
【8】BACKER L C, CARMICHAEL W, KIRKPATRICK B, et al. Recreational exposure to low concentrations of microcystins during an algal bloom in a small lake［J］. Marine Drugs, 2008,6(2):389-406.
【9】虞锐鹏,陶冠军,贡小清,等.高效液相色谱-质谱联用方法测定背角无齿蚌体内微囊藻毒素［J］.分析测试学报, 2007,26(5):671-674.
【10】BARCO M, FLORES C, JOSEP R, et al. Determination of microcystin variants and related peptides present in a water bloom of Plank tothrix (oscillatoria) rubescens in a spanish drinking water reservoir by LC/ESI-MS［J］. Toxicon, 2004,44(8):881-886.
【11】周伟杰,刘萍,李雪,等.太湖淡水螺体内微囊藻毒素污染动态研究［J］.实用预防医学, 2012,19(3):349-351.
【12】HARADA K I, MATSUURA K, SUZUKI M, et al. Isolation and characterization of the minor components associated with microcystins LR and RR in the cyanobacterium (blue-green algae)［J］. Toxicon, 1990,28(1):55-64.
【13】刘飞,王勇为.高效液相色谱-串联质谱法测定鲫鱼中的微囊藻毒素［J］.环境化学, 2010,29(4):785-786.
【14】YANG Bo, XU Jin-zhong, DING Tao, et al. A novel method to detect seven microcystins in hard clam and corbicula fluminea by liquid chromatography-tandem mass spectrometry［J］. Journal of Chromatography B, 2009,877(29):3522-3528.
【15】OTT J L, CARMICHAEL W W. LC/ESI/MS method development for the analysis of hepatotoxic cyclic peptide microcystins in animal tissues［J］. Toxicon, 2006,47(7):734-741.
【16】闫建秀,虞锐鹏,汤坚,等.固相萃取-反相高效液相色谱法检测太湖蛳螺中微囊藻毒素［J］.安全与检测, 2008,24(5):92-95.
【17】DAI Ming, XIE Ping, LIANG Gao-dao, et al. Simultaneous determination of microcystin-LR and its glutathione conjugate in fish tissues by liquid chromatography-tandem mass spectrometry［J］. Journal of chromatography B, 2008,862(12):43-50.
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