UPLC-MS/MS快速测定甘蓝类蔬菜中活性成分莱菔硫烷  

Determination of Bioactive Compound Sulforaphane in Brassica Vegetables by UPLC-MS/MS

作　　者：李占省[1] 刘玉梅[1] 方智远[1] 杨丽梅[1] 庄木[1] 张扬勇[1] 李凌云 吕红豪[1] 孙培田[1] 

机构地区：[1]中国农业科学院蔬菜花卉研究所,北京100081 [2]农业部蔬菜品质监测检验中心,北京100081

出　　处：《安徽农业科学》2015年第36期1-3,6,共4页Journal of Anhui Agricultural Sciences

基　　金：国家自然科学基金项目(31372067);现代农业产业技术体系建设专项资金项目(CARS-25-A);国家科技支撑计划课题(2013BAD01B04);国家高新技术发展计划(2012AA100105);农业部园艺作物生物学与种质创制重点实验室;中国农业科学院科技创新工程(CAAS-ASTIP-IVFCAAS)

摘　　要：[目的]为了建立快速测定甘蓝类蔬菜（甘蓝、青花菜、芥蓝、苤蓝）中莱菔硫烷活性成分的方法。[方法]采用超高效液相色谱-串联质谱UPLC-MS/MS,快速测定甘蓝类蔬菜中莱菔硫烷含量。[结果]采用酶解-乙酸乙酯萃取法提取莱菔硫烷,Waters BEH反相C18（2.1 mm×50.0 mm,1.7μm）分离,质谱采用电喷雾正离子ESI（＋）电离,多反应监测扫描模式（MRM）检测。在4种甘蓝类蔬菜（可食性器官）中均检测到莱菔硫烷成分,在0.1～20.0μg/L范围内线性关系良好,相关系数为0.999 4,相对标准偏差（RSD,n=6）为2.4%,检出限（LOD,S/N=3）为0.06～0.15μg/L,定量下限（LOQ,S/N=10）为0.3～0.4μg/L。[结论]该方法准确可靠,能够快速检测甘蓝类蔬菜中莱菔硫烷抗癌活性成分。[Objective] The aim was to establish a rapid method for the determination of sulforaphane in Brassica vegetables（ cabbage,broccoli,Chinese kale and kohlrabi）. [Method] Ultra high performance liquid chromatography coupled with tandem mass spectrometry（ UPLC-MS /MS） was developed to determine the sulforaphane content in Brassica vegetables. [Result]Sulforaphane was extracted by the solvent of ethyl acetate. The compound was separated on Waters BEH C18（ 2. 1 mm × 50. 0 mm,1. 7 μm） column,and mass spectrum was analyzed by electro spray ionization in positive mode ESI（ ＋） under multiple reaction monitoring（ MRM） mode. Brassica vegetables contained sulforaphane,and the calibration curve showed a good linear in the range of 0. 1- 20. 0 μg / L with the correlation coefficient of 0. 999 4. The relative standard deviation（ RSD） was 2. 4%（ n = 6）. The detection limit（ LOD,S / N = 3） was in range of 0. 06-0. 15 μg / L,and the quantitation limit（ LOQ,S / N =10） was 0. 3-0. 4 μg / L. [Conclusion] The method was accurate and reliable,so it could quickly detect the anti-cancer compound of sulforaphane in Brassica vegetables.

关 键 词：超高效液相色谱-串联质谱法 甘蓝类蔬菜 抗癌成分 莱菔硫烷 

分 类 号：S635[农业科学—蔬菜学]