超高效液相色谱法快速测定贝类中的软骨藻酸残留
UHPLC Rapid Determination of Residual Domoic Acid in Shellfishes
摘 要
利用超高效液相色谱快速测定贝类中的软骨藻酸残留。样品经甲醇(1+1)溶液提取,采用Oasis MAX固相萃取柱对提取液进行净化后,在Waters ACQUITY UPLC BEH C18色谱柱上分离,以乙腈-0.1%(体积分数)三氟乙酸(13+87)混合液为流动相进行洗脱,紫外检测波长为242 nm。软骨藻酸的线性范围为0.1~10.0 mg·L-1,测定下限(10S/N)为0.2 mg·kg-1。加标回收率在76.8%~91.2%之间,测定值的相对标准偏差(n=6)在11%~16%之间。
软骨藻酸
贝类
UHPLC
Domic acid
Shellfishes
Abstract
UHPLC was applied to the determination of residual domoic acid in shellfishes. The sample was extracted with methanol (1+1) solution. The extract was purified on Oasis MAX solid extraction column and the supernatant was separated on Waters ACQUITY UPLC BEH C18 chromatographic column with acetonitrile-0.1% (φ) trifluoroacetic acid solution (13+87) as the mobile phase for isocratic elution. UV-detection was made at the wavelength of 242 nm. The linearity range of domoic acid was 0.1-10.0 mg·L-1, with the lower limit of determination (10S/N) of 0.2 mg·kg-1. Recovery rates obtained by standard addition method were in the range of 76.8%-91.2%, and RSDs (n=6) were in the range of 11%-16%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx201510010
所属栏目 工作简报
基金项目
收稿日期 2014/9/12
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备注褚莹倩(1987-),女,辽宁本溪人,硕士研究生,研究方向为生物毒素。
引用该论文: CHU Ying-qian,XIE Ying,CHEN Xi,CUI Han,ZHANG Xiao-lin,HUANG Da-liang. UHPLC Rapid Determination of Residual Domoic Acid in Shellfishes[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(10): 1396～1399
褚莹倩,谢瀛,陈溪,崔晗,张晓林,黄大亮. 超高效液相色谱法快速测定贝类中的软骨藻酸残留[J]. 理化检验－化学分册, 2015, 51(10): 1396～1399
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参考文献
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【7】GB/T 5009.198-2003贝类 记忆丧失性贝类毒素软骨藻酸的测定［S］.
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【10】TOR E R, PUSCHNER B, WHITEHEAD W E. Rapid determination of domoic acid in serum and urine by liquid chromatography-electrospray tandem mass spectrometry［J］. Journal of Agricultural and Food Chemistry, 2003,51(7):1791-1796.
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【12】YU Feng-yih, LIU Biing-hui, WU Ting-shuan, et al. Development of a sensitive enzyme-linked immunosorbent assay for the determination of domoic acid in shellfish［J］. Journal of Agricultural and Food Chemistry, 2004,52(17):5334-5339.
【13】刘淑娟,赵晓祥,王茜,等.软骨藻酸快速检测方法技术研究［J］.上海交通大学学报:农业科学版, 2014,32(2):10-14.
【14】SMITH D, KITTS D D. Enzyme immunoassay for the determination of domoic acid in mussel extracts［J］. Journal of Agricultural and Food Chemistry, 1995,43(2):367-371.
【15】ZHAO Jian-ying, THIBAULT P, QUILLIAM M A. Electrophoresis-analysis of domoic acid and isomers in seafood by capillary electrophoresis［J］. Electrophoresis, 1997,18:268-276.
【16】ZHOU Wen-hui, GUO Xiu-chun, ZHAO Heng-qiang, et al. Molecularly imprinted polymer for selective extraction of domoic acid from seafood coupled with high-performance liquid chromatographic determination［J］. Talanta, 2011,84:777-782.
【17】卫锋,程昉,宫静宏,等.高效液相色谱法测定贝类中的软骨藻酸［J］.色谱, 2001,19(3):248-250.
【18】吉薇,郑洁莹,曾雪萍,等.南海海域软骨藻酸(DA)贝类毒素的HPLC方法检测［J］.现代食品科技, 2011,27(1):120-122.
【19】周秀锦,周向阳,郑斌,等.HPLC法快速检测记忆缺失性贝毒软骨藻酸［J］.浙江海洋学院学报:自然科学版, 2012,31(5):211-214.
【2】吴冬梅,张雁秋,程伟,等.软骨藻酸神经毒性作用机制研究进展［J］.生态毒理学报, 2013,8(1):1-6.
【3】JEFFERY B, BARLOW T, MOIZER K, et al. Amnesic shellfish poison［J］. Food and Chemical Toxicology, 2004,42:545-557.
【4】CLAYDEN J, READ B, HEBDITCH K R. Chemistry of domoic acid, isodomoic acids, and their analogues［J］. Tetrahedron, 2005,61:5713-5724.
【5】REGUEIRO J, LVAREZ G, MAURIZ A, et al. High throughput analysis of amnesic shellfish poisoning toxins in bivalve molluscs by dispersive solid-phase extraction and high-performance liquid chromatography using a monolithic column［J］. Food Chemistry, 2011,127:1884-1891.
【6】马荣桧,高彦,万进,等.贝类毒素及检测技术的研究现状［J］.食品研究与开发, 2013,34(22):104-108.
【7】GB/T 5009.198-2003贝类 记忆丧失性贝类毒素软骨藻酸的测定［S］.
【8】CIMINIELLO P, DELL′AVERSANO C, FATTORUSSO E, et al. Hydrophilic interaction liquid chromatography/mass spectrometry for determination of domoic acid in Adriatic shellfish［J］. Rapid Communications in Mass Spectrometry, 2005,19:2030-2038.
【9】REGUEIRO J, MARTIN E, LVAREZ G, et al. Sensitive determination of domoic acid in shellfish by on-line coupling of weak anion exchange solid-phase extraction and liquid chromatography-diode array detection-tandem mass spectrometry［J］. Food Chemistry, 2011,129:672-678.
【10】TOR E R, PUSCHNER B, WHITEHEAD W E. Rapid determination of domoic acid in serum and urine by liquid chromatography-electrospray tandem mass spectrometry［J］. Journal of Agricultural and Food Chemistry, 2003,51(7):1791-1796.
【11】GARTHWAITE I, ROSS K M, MILES C O, et al. Polyclonal antibodies to domoic acid, and their use in immunoassays for domoic acid in sea water and shellfish［J］. Natural Toxins, 1998,6:93-104.
【12】YU Feng-yih, LIU Biing-hui, WU Ting-shuan, et al. Development of a sensitive enzyme-linked immunosorbent assay for the determination of domoic acid in shellfish［J］. Journal of Agricultural and Food Chemistry, 2004,52(17):5334-5339.
【13】刘淑娟,赵晓祥,王茜,等.软骨藻酸快速检测方法技术研究［J］.上海交通大学学报:农业科学版, 2014,32(2):10-14.
【14】SMITH D, KITTS D D. Enzyme immunoassay for the determination of domoic acid in mussel extracts［J］. Journal of Agricultural and Food Chemistry, 1995,43(2):367-371.
【15】ZHAO Jian-ying, THIBAULT P, QUILLIAM M A. Electrophoresis-analysis of domoic acid and isomers in seafood by capillary electrophoresis［J］. Electrophoresis, 1997,18:268-276.
【16】ZHOU Wen-hui, GUO Xiu-chun, ZHAO Heng-qiang, et al. Molecularly imprinted polymer for selective extraction of domoic acid from seafood coupled with high-performance liquid chromatographic determination［J］. Talanta, 2011,84:777-782.
【17】卫锋,程昉,宫静宏,等.高效液相色谱法测定贝类中的软骨藻酸［J］.色谱, 2001,19(3):248-250.
【18】吉薇,郑洁莹,曾雪萍,等.南海海域软骨藻酸(DA)贝类毒素的HPLC方法检测［J］.现代食品科技, 2011,27(1):120-122.
【19】周秀锦,周向阳,郑斌,等.HPLC法快速检测记忆缺失性贝毒软骨藻酸［J］.浙江海洋学院学报:自然科学版, 2012,31(5):211-214.
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