贝类产品中软骨藻酸的HPLC检测方法  

Rapid Detection of Domoic Acid in Shellfishes by HPLC

作　　者：高治昊 林郑忠[1] 陈晓梅[1] 黄志勇[1] 

机构地区：[1]集美大学食品与生物工程学院,福建厦门361021

出　　处：《集美大学学报（自然科学版）》2015年第4期255-259,共5页Journal of Jimei University：Natural Science

基　　金：国家自然科学基金资助项目(21305050);福建省科技计划重点项目(2012Y0052;2014Y0045);厦门市科技计划项目(3502Z20143018);集美大学创新团队基金资助项目(2010A007)

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,5μm）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20μL,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.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 con-clusion, the established method can be used to detect trace domoic acid in shellfish samples rapidly without further purification treatment by SPE columns.

关 键 词：软骨藻酸 高效液相色谱 贝类 快速检测 

分 类 号：TS207.3[轻工技术与工程—食品科学]