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贝类产品中软骨藻酸的HPLC检测方法
引用本文:高治昊,林郑忠,陈晓梅,黄志勇.贝类产品中软骨藻酸的HPLC检测方法[J].集美大学学报(自然科学版),2015,0(4):255-259.
作者姓名:高治昊  林郑忠  陈晓梅  黄志勇
作者单位:(集美大学食品与生物工程学院,福建 厦门 361021)
基金项目:国家自然科学基金资助项目,福建省科技计划重点项目,厦门市科技计划项目,集美大学创新团队基金资助项目
摘    要:建立了高效液相色谱测定贝类产品中软骨藻酸的检测方法,具体过程为:样品先经甲醇浸提后,再用甲醇-水(V(甲醇)∶V(水)=1∶1)提取2次,合并提取液后用Zorbax SB300-C18柱(2.1 mm×250 mm,5 μm)进行分离,以乙腈-0.2%磷酸水溶液(含0.1%三乙胺)(V(乙腈)∶V(磷酸水溶液)=12∶88)为流动相于室温下等度洗脱,流速为0.25 mL/min,进样量20 μL,检测波长为242 nm.结果表明,在建立的提取方法和色谱条件下,软骨藻酸从复杂的样品基体中被分离出来,在0.02~1.0 mg/L质量浓度范围内具有良好的线性关系(r>0.999),样品的平均加标回收率为108%,测量方法的RSD为3.5%(n=6),检出限为23.5 ng/g.所建立的检测方法可适用于对贝类产品中软骨藻酸的快速检测.

关 键 词:软骨藻酸  高效液相色谱  贝类  快速检测

Rapid Detection of Domoic Acid in Shellfishes by HPLC
GAO Zhi-hao,LIN Zheng-zhong,CHEN Xiao-mei,HUANG Zhi-yong.Rapid Detection of Domoic Acid in Shellfishes by HPLC[J].the Editorial Board of Jimei University(Natural Science),2015,0(4):255-259.
Authors:GAO Zhi-hao  LIN Zheng-zhong  CHEN Xiao-mei  HUANG Zhi-yong
Affiliation:(College of Food and Biological Engineering,Jimei University,Xiamen 361021,China)
Abstract:A rapid detection method by high performance liquid chromatography (HPLC) was developed to determine the concentrations of domoic acid in different species of shellfish.After extraction by methanol and methanol-water (1∶1,V/V),the sample was separated using a Zorbax SB300-C18 chromatographic column (2.1 mm×250 mm,5 μm),and was eluted with acetonitrile-0.2% phosphoric acid solution (containing 0.5% triethylamine) (12∶88,V/V) at room temperature.The flow rate was set as 0.25 mL/min.20 μL of sample was individually injected,and the detection wavelength was 242 nm.The results showed that domoic acid can be well separated from the sample matrix within 8 min with a linear range of 0.02~1.0 mg/L(r>0.999).The average recovery as tested by adding standards was 108%,and the RSD was 3.5%(n=6).The detection limit estimated with three folds of standard deviations was 23.5 ng/g.In conclusion,the established method can be used to detect trace domoic acid in shellfish samples rapidly without further purification treatment by SPE columns.
Keywords:domoic acid  HPLC  shellfish  rapid detection
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