蜂王浆中脂肪酸的高效液相色谱-质谱法检测  

Determination of fatty acids in royal jelly by liquid chromatography-mass spectrometry

作　　者：刘善菁 陈磊[2] 张睿[2] 吴斌[2] 陈惠兰[2] 张晓燕[2] 费晓庆[2] 杨功俊[1] 

机构地区：[1]中国药科大学药学院,南京211198 [2]江苏出入境检验检疫局食品实验室,南京210001

出　　处：《扬州大学学报（自然科学版）》2015年第2期40-44,共5页Journal of Yangzhou University：Natural Science Edition

基　　金：国家自然科学基金资助项目(21275162);江苏省"青蓝工程"资助项目

摘　　要：建立了一种高效液相色谱-四级杆/飞行时间质谱法检测蜂王浆中6种脂肪酸.样品经水溶液溶解和甲醇沉淀蛋白后,以C18反相色谱柱为分析柱,乙腈和φ（甲酸）=0.1%的水溶液为流动相,通过梯度洗脱对8-羟基辛酸、10-羟基-2-癸烯酸、癸二酸、10-羟基癸酸、2-十二碳烯二酸和十二烷二酸等6种脂肪酸进行分离,并采用四级杆/飞行时间质谱检测器对其进行定性和定量分析.定量分析结果显示,方程线性相关系数（r2）为0.997 5~0.999 7,定量限为0.10~1.0mg·L-1,检出限为0.050~0.20mg·L-1,加标回收率为82.9%~107.0%,相对标准偏差为0.9%~4.9%.用该方法对采自我国不同地区137份蜂王浆样品进行分析,初步确定合格蜂王浆中10-羟基-2-癸烯酸、10-羟基癸酸和8-羟基辛酸3种脂肪酸的含量,并建议在现行国家标准的基础上增加10-羟基癸酸和8-羟基辛酸作为蜂王浆质量评价的指标.A liquid chromatography-quadrupole/time of flight mass spectrometry method was developed for determination of 8-hydroxyoctanoic acid,10-hydroxy-2-decenoic acid,sebacic acid,10-hydroxydecanic acid,2-dodecenedioic acid,dodecanedioic acid in royal jelly.The samples were dissolved in formic acid solution and deproteinized by methanol.C18 reversed phase column was used for separation with acetonitrile andφ（formic acid）=0.1% solution as mobile phase by gradient elution program.The electrospray ionization was operated in negative mode.Full mass scan and target MS/MS in high resolution mode were used in qualitative and quantitative analysis.Under the optimum conditions,the 6fatty acids performed good linearity with correlation coefficient（r2）of0.997 5~0.999 7.The limit of quantitation（LOQ）and limit of detection（LOD）limits were in the range of 0.10~1.0mg·L-1 and of 0.050~0.20mg·L-1,respectively.The average recoveries of6 fatty acids were in the range of 82.9% ~107.0% with relative standard deviations of 0.9%~4.9%.The method has been used to analyze 137 royal jelly samples from different area of China and the contents of 8-hydroxyoctanoic acid,sebacic acid and 10-hydroxydecanic acid in these samples were determined.The contents of 10-hydroxydecanic acid and 8-hydroxyoctanoic acid were suggested as supporting parameters for quality evaluation of royal jelly based on the current national standards.

关 键 词：蜂王浆 10-羟基-2-癸烯酸 10-羟基癸酸 8-羟基辛酸 四级杆-飞行时间质谱 液相色谱 

分 类 号：O657.63[理学—分析化学] S896.3[理学—化学]