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高效液相色谱法测定卤虫无节幼体中精胺含量
王新星1,2, 于朝磊1,3, 马静1,3, 常青1
1.农业部海洋渔业可持续发展重点实验室,中国水产科学研究院黄海水产研究所 青岛 266071;2.青岛科技大学化学与分子工程学院,266042;3.上海海洋大学水产与生命学院,201306
摘要:
本研究建立了高效液相色谱法测定卤虫无节幼体中精胺含量的方法。样品经5%三氯乙酸溶液提取,提取液采用丹璜酰氯柱前衍生,以甲醇-水为流动相,经C18反相色谱柱分离后用紫外检测器检测。精胺的线性范围为0.1~103μg/ml,线性相关系数0.9999,检出限为0.06μg/ml。3个添加浓度(0.1、1.0和5.0μg/ml)的平均回收率范围为86.3%~96.3%,相对标准偏差皆小于5%。采用此方法对卤虫中精胺进行检测,其精胺含量为0.077mg/g。本方法具有分析时间短,线性范围宽,灵敏度和精密度高等优点,适合于卤虫中精胺的检测。
关键词:  精胺  卤虫  高效液相色谱
DOI:10.11758/yykxjz.20130617
分类号:
基金项目:国家自然科学基金项目(31101913)
Determination of spermine in brine shrimp by HPLC
Abstract:
An analytical method was established for the determination of spermine in brine shrimp by high performance liquid chromatography (HPLC) with ultraviolet detector. Spermine in brine shrimp samples was extracted with a mixture of 5% TCA, then derived with dansyl chloride, followed by separation via the C18 RP-HPLC column with methanol-water. Under the optimal conditions, spermine showed good linear relationship in the range of 0.1~103μg/ml and the correlation coefficient (R2) was 0.9999. At the spiked levels of 0.1, 1.0 and 5.0μg/ml, the average recoveries were 86.3%~96.3% with the relative standard deviations less than 5%. The minimum detection concentration was 0.06μg/ml. The overall process was successfully applied to identify and quantify spermine in brine shrimp, and the value was 0.077mg/g. The method is sensitive, rapid and precise.
Key words:  Spermine  Brine shrimp  HPLC