高效液相色谱-串联质谱法测定紫苏籽油中11种酚类化合物  

Simultaneous Determination of 11 Phenolic Compounds in Perilla oil by High Performance Liquid ChromatographyTandem Mass Spectrometry

作　　者：吴娆[1,2] 马飞[1,3] 张良晓[1,4,3] 李培武[1,5,4,3] 张文[1,3] 张奇[1,5] 李光明[1,2,3] 

机构地区：[1]中国农业科学院油料作物研究所,武汉430062 [2]农业部油料作物生物学与遗传改良重点实验室,武汉430062 [3]农业部油料及制品质量监督检验测试中心,武汉430062 [4]农业部油料作物风险评估重点实验室,武汉430062 [5]农业部生物毒素检测重点实验室,武汉430062

出　　处：《分析化学》2015年第10期1600-1606,共7页Chinese Journal of Analytical Chemistry

基　　金：国家科技支持计划课题(No.2012BAK08B03);国家自然科学基金(Nos.21205118,31201447);国家农产品质量安全风险评估重大项目(Nos.GJFP2015006,GJFP201502-03),农业部;财政部专项课题“国家油菜现代产业技术体系建设”(No.CARS-13)资助~~

摘　　要：基于新型富集材料磁性羧基化多壁碳纳米管与高效液相色谱-串联质谱,建立了紫苏籽油中11种酚类化合物同时分离与检测的方法。对影响富集分离效果的重要因素,如流动相、流动相中酸的添加量、流速、进样量及碰撞能量等条件进行了详细优化。在优化条件下,11种酚类化合物线性关系良好,相关系数为0.993~0.999,检出限（LOD,S/N=3）和定量限（LOQ,S/N=10）分别在0.02~0.70 ng/m L,0.06~2.0 ng/m L范围内,以50和500 ng/m L添加浓度水平进行方法学验证,回收率为79.6%~121.5%,相对标准偏差为0.06%~13.2%。将本方法应用于紫苏籽油样品的分析,其含量在7.32~68.6 ng/g之间。结果表明,本方法操作简单、准确可靠,适用于紫苏籽油等植物油中酚类化合物定量分析。A new separation and analysis method was developed to simultaneously detect 11 phenolic compounds in edible oil based on the multi-walled carbon nanotube modified with carboxyl（ MWCNTs-COOH）and high performance liquid chromatography-tandem mass spectrometry（ HPLC-MS / MS）. Experimental conditions,including mobile phase,addictive acids,flow rate as well as injection parameters,were fully optimized. Under the optimal conditions, 11 phenolic compounds showed good linearity over tested concentration ranges with the correlation coefficients from 0. 993 to 0. 999. The limits of detection（ LOD） and limits of quantitation（ LOQ） were in the range of 0. 02- 0. 70 ng / m L and 0. 06- 2. 0 ng / m L,respectively.The average recoveries of two concentration levels ranged from 79. 6% to 121. 5% with the relative standard deviations（ RSD） from 0. 06% to 13. 2%. This method was employed to detect 11 phenolic compounds in Perilla oils. The content ranges of phenolics in perilla oils were from 7. 32 ng / g to 68. 6 ng / g. The results indicated that the method was accurate and reliable,and suitable for the analysis of phenols in edible oils.

关 键 词：紫苏籽油 酚类化合物 磁固相萃取法 高效液相色谱-串联质谱 

分 类 号：TS227[轻工技术与工程—粮食、油脂及植物蛋白工程] O657.63[轻工技术与工程—食品科学与工程]