分析化学2011，Vol.39Issue(1)：57-61,5.
高效液相色谱-三重四级杆质谱分析海洋甲壳动物淋巴和肌肉中的20-羟基蜕皮酮
Determination of 20-Hydroxyecdysone in Several Marine Crustaceans by Liquid Chromatography-Mass Spectrometry
摘要
Abstract
A method based on high performance liquid chromatography coupled with electronspray ionization/triple quadrupole mass spectrometry(HPLC/QqQ-MS) has been established for the determination of 20-hydroxyecdysone in the haemolymph of Portunus trituberculatus and in the muscle of crustacean (Portunus trituberculatus, Palaernon carincauda Holthuis and Oratosquilla oratoria ).Homobrassinolide was utilized as internal standard. The mass spectrometry was performed in positive mode, using precursor ions at m/z 445.2 and 459.4 as quantitative ions for 20-hydroxyecdysone and 22(S), 23 (S)-homobrassinolide, respectively. The results showed that 20-hydroxyecdysone and 22 (S), 23(S)-homobrassinolide were separated with high efficiency in the selective reaction monitoring (SRM) mode on Hypersil Gold C18column. Linearity of the method was good with correlation coefficients(R 2) of 0. 9978 in the range of 0-50 μg/L. The detection limit was 0.03 μg/L. The recoveries varied from 91.8％ to 99.2％ for the haemolymph and 85.7％ to 91.2％ for the muscle with the relative standard deviations(RSDs) from 7.3％ and 7.1％, respectively. Using this method, 20-hydroxyecdysone in the haemolymph of Portunus trituberculatus collected in Ningbo China, has been determined with content ranged from 2.43 to 2.8( μg/L; the concentration of 20-Hydroxyecdysone in the muscle of crustaceans( Portunus trituberculatus , Palaernon carincauda Holthuis and Oratosquilla oratoria) were determined from 4.8 to 9. 6 ng/g. The method is a powerful tool for comprehensive analysis of biological sample with exclusive selectivity and excellent sensitivity.关键词
20-羟基蜕皮酮/甲壳动物/液相色谱-三重四级杆质谱Key words
20-Hydroxyecdysone/ Crustacean/ High performance liquid chromatography-electrospray ionization-triple quadrupole mass spectrometry引用本文复制引用
赵鹏,徐继林,亓一舟,陈娟娟,朱冬发,严小军..高效液相色谱-三重四级杆质谱分析海洋甲壳动物淋巴和肌肉中的20-羟基蜕皮酮[J].分析化学,2011,39(1):57-61,5.基金项目
本文系教育部长江学者与创新团队项目(No.IRT0734)、国家自然科学基金(No.40976098)、国家科技支撑计划(No.2007BAD43807)和宁波大学工宽诚幸福基金资助 （No.IRT0734）
