柱前衍生HPLC-MS法测定黑果枸杞果实中脂肪酸  

Determination and analysis of fatty acids in Lycium ruthenicum Murr fruits by HPLC-MS with precolumn derivatization

作　　者：胡娜[1,2,3] 索有瑞[1,2] 韩丽娟[1,3] 索有芳 尤进茂[1] 

机构地区：[1]中国科学院西北高原生物研究所,西宁810001 [2]青海大学农林科学院,西宁810016 [3]中国科学院大学,北京100049 [4]青海省环境监测中心站,西宁810007

出　　处：《分析试验室》2014年第6期698-701,共4页Chinese Journal of Analysis Laboratory

基　　金：科技部星火计划项目(2011GA870007)资助

摘　　要：采用柱前衍生荧光检测高效液相色谱-大气压化学电离源/质谱联用技术对黑果枸杞果实中的脂肪酸成分进行分析。经2-（11-H-苯-a-咔唑）乙基对甲苯磺酸酯荧光衍生试剂对脂肪酸进行柱前衍生,梯度洗脱分离,荧光检测,外标法定量和在线质谱鉴定,建立了同时测定20种脂肪酸含量的方法,并运用此方法对黑果枸杞果实中的脂肪酸进行了分析。结果表明。检测限可以达到0.42～1.84 ng/mL。黑果枸杞果实中主要含有不饱和脂肪酸,其含量约占整个脂肪酸总量的64%,其中不饱和脂肪酸种类主要是C18∶1（油酸）,C18∶2（亚油酸）和少量的C18∶3（亚麻酸）;饱和脂肪酸主要是以C16（棕榈酸）,C18（硬脂酸）,C20（花生酸）和C22（山嵛酸）为主,另外还含有少量的C12（月桂酸）,C14（肉豆蔻酸）,C17（珠光脂酸）,C23（二十三酸）和C24（木蜡酸）。本研究可以为黑果枸杞在食品、医药和保健方面的进一步开发应用提供可靠的科学依据。In the present study, fatty acids in fruits of Lycium ruthenicum Murr were analyzed by HPLC - FLD - APCI/MS with pre - column derivatization and fluorescence detection . A method for the determination of the absolute contents of 20 kinds of fatty acids by pre - column derivatization with 2 - （ 11H - benzo [ a ] carbazol - 11 - yl） ethyl 4 - methylbenzenesulfonate （BCETS） as a derivatization reagent, gradient elution, fluorescence detection, external standard method and online MS identification was established. The method was successfully employed to analyze fatty acids in the fruits of Lycium ruthenicum Murr. The results show that the method has high sensitivity, selectivity, good reproducibility and applicability. The limits of detection were in the range of 0. 42- 1.84 ng/mL. The main fatty acids in the fruits of Lycium ruthenicum Murr are unsaturated fatty acids including C18： 1, C18：2 and C18： 3, the percentage of which could reach 64%. The primary saturated fatty acids are C16, C18, C20 and C22, and there are little amounts of C12, C14, C17, C23 and C24. This research can provide reliably scientific basis for its development and application in food, medicine and health products.

关 键 词：黑果枸杞 脂肪酸 柱前衍生 高效液相色谱-大气压化学电离源 质谱联用技术 

分 类 号：O657.63[理学—分析化学]