摘要
目的：建立高灵敏度检测河豚毒素的高效液相色谱一荧光法。方法：采用柱后衍生高效液相色谱-荧光法检测河豚毒素含量，以庚烷磺酸钠为离子对试剂，应用反相离子对液相色谱分离河豚毒素，采用在线柱后衍生系统，在110％高温和4mol／LNaOH强碱条件下，将河豚毒素衍生化成具有荧光特性的C9碱，荧光检测器定量检测。结果：河豚毒素在0．408—102．00μg／ml范围内呈良好的线性相关，相关系数r=0．9999；方法的检测限为0．41 ng；定量限为0．81 ng；精密性试验相对标准偏差为0．29％；重复性试验相对标准偏差为1．87％；平均回收率为99．70％，标准偏差为1．87％。结论：本方法简单、可靠、灵敏，可用于微量河豚毒素的精确定量分析。
Objctive：To study on quantitative detection of tetrodotoxin. Methods：Trx was detected by post column derivation HPLC and separated by reverse phase ion - pair liquid chromatography, of which ion - pair reagent was heptanesulfonic acid sodium salt, then heated with 4 mol/L NaOH at 110℃ in on - line derivation system. It was converted to C9 - base with fluorescence characteristic, quantified by fluorescence detector. Results：Good linearity was observed： the linear range was 0. 40512 - 101.28μg/ml and linear relationship r = 1. 000. The limits of detection were 0. 41 ng and the limits of quantification were 0. 81 ng. The RSD of precision and repetition was 0. 29% and 1.87%. Average recovery was 99. 70%, RSD was 1.87%. Conclusion： This method is simple, accurate and sensitive. It is suitable for detection of TTX.
出处
《中国卫生检验杂志》
CAS
2009年第2期261-262,270,共3页
Chinese Journal of Health Laboratory Technology
基金
基本科研业务费资助专项项目(海三科2007005
海三科2008019)
