仿刺参体腔液中皮质醇检测方法研究  

Detection Method of Hydrocortisone in Coelomic Fluid of Sea Cucumber Apostichopus japonicus

作　　者：刘桂英[1] 田金[1] 肖瑶 吴金浩[1] 宋伦[1] 高颖[1] 王志松[1] LIU Guiying;TIAN Jin;XIAO Yao;WU Jinhao;SONG Lun;GAO Ying;WANG Zhisong(Liaoning Ocean and Fisheries Science Research Institute, Dalian 116023, China)

机构地区：[1]辽宁省海洋水产科学研究院,辽宁大连116023

出　　处：《水产科学》2020年第4期591-595,共5页Fisheries Science

基　　金：国家重点研发计划项目(2018YFD0900105);辽宁省科学事业公益研究基金资助项目(20170036);辽宁省重点研发计划项目(2018228004);辽宁省海洋与渔业科研项目(201828,201824)。

摘　　要：建立了3龄仿刺参和幼参体腔液中皮质醇的超高效液相色谱—串联质谱的检测方法。样品采用乙腈-0.2%甲酸溶液均质振荡、超声提取,用Captiva EMR-Lipid固相萃取柱净化,BEH C-18色谱柱分离,采用超高效液相色谱—串联质谱仪进行测定。试验结果表明,方法的检出限为0.11μg/L,定量限为0.35μg/L,在空白样品中分别添加皮质醇质量浓度为20、40、100μg/L,其回收率均为77%~105%,该方法基质干扰小,准确,易操作,能够满足仿刺参体腔液中痕量皮质醇的测定。In this paper,a ultra-performance liquid chromatography-linear ion trap mass spectrometry(UPLC-MS)method was established for the detection of hydrocortisone in coelomic fluid of juvenile and 3 year old sea cucumber Apostichopus japonicus.Extraction conditions and purification methods were optimized.Samples were extracted with 0.2%formic acid acetonitrile solution,and the extract was subjected to chromatographic separation on Captiva EMR-lipid solidphase extraction column.Quantification of the analytes was achieved by UPLC-MS using the external standard method,with the limit of detection(LOD)of 0.11μg/kg,and the limit of quantification(LOQ)of 0.35μg/kg.The average recoveries of hydrocortisone in blank samples at spiked levels of 20,40,and 100μg/L were ranged from 77%to 105%.This method had the advantages of small matrix interference and accurate,which can satisfy detection of hydrocortisone in sea cucumber.

关 键 词：皮质醇 超高效液相色谱—串联质谱 固相萃取 固相萃取柱 

分 类 号：S912[农业科学—水产科学]