超高效液相色谱-串联质谱法测定32种蔬菜中萝卜硫素  

Determination of sulforaphane in 32 vegetables by ultra-high performance liquid chromatography tandem mass spectrometry

作　　者：陈淼 蒲杰 向维 赵雪雯 曾静 CHEN Miao;PU Jie;XIANG Wei;ZHAO Xuewen;ZENG Jing(School of Phannacy,Southwest Medical University,Luzhou 646000)

机构地区：[1]西南医科大学药学院,泸州646000

出　　处：《分析试验室》2021年第1期21-24,共4页Chinese Journal of Analysis Laboratory

基　　金：国家级大学生创新创业训练计划项目(201810632063)资助。

摘　　要：建立了超高效液相色谱-串联质谱(UHPLC-MS/MS)测定蔬菜中萝卜硫素的方法,并测定了32种常见蔬菜的萝卜硫素含量。取蔬菜冻干粉,利用内源黑芥子酶在p H 5的H3PO4缓冲液条件下酶解,酶解液经冷冻干燥后用乙酸乙酯提取,经减压浓缩后用50%乙腈-水(V/V)复溶。复溶液采用Shimpack XR-ODS II色谱柱,以0.1%(V/V)甲酸-水溶液和0.1%(V/V)甲酸-乙腈(95:5,V/V)为流动相进行梯度洗脱;采用电喷雾离子源(ESI),在正离子模式下进行多反应监测(MRM)扫描。结果表明,萝卜硫素在0.210~105 ng/mL范围内线性关系良好,检出限和定量限分别为52.5 pg/mL和210 pg/mL。经检测,西兰花中萝卜硫素的含量最高,其次为莲花白、花椰菜、紫甘蓝等十字花科植物。非十字花科蔬菜中,大葱的萝卜硫素含量最高。A method for the determination of sulforaphane in vegetables by ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)was established for the quantitative analysis of sulforaphane in 32 vegetables.The lyophilized vegetable powder was enzymatically hydrolyzed by endogenous black myrosinase in phosphate buffer solution(pH 5).The hydrolyzed product was extracted with ethyl acetate after freeze-drying.The extract was concentrated under vacuum and then dissolved with 50%aqueous acetonitrile.Shimadzu Shim-pack XR-ODS II column(2.1 mm×100 mm,2.7 mm,100 A)was used for the separation.The 0.1%(V/V)formic acid-water and 0.1%(V/V)formic acid-acetonitrile were used as the mobile phase,and a universal gradient was adopted for the elution.Electrospray ionization source(ESI)was employed with positive ion mode for multiple reaction monitor(MRM).The results showed a satisfied linearity for sulforaphane amount in the range of 0.210-105 ng/m L(R~2=1),and the detection limit and quantification limit were 52.5 pg/m L and 210 pg/m L,respectively,demonstrating the favourable accuracy and precision of this method.As the determination results,the content of sulforaphane in broccoli is the highest in cruciferous plants,followed by cabbage,cauliflower and purple cabbage.Besides,the content of sulforaphane in scallions were the highest in non-cruciferous vegetables.

关 键 词：超高效液相色谱串联质谱法 萝卜硫素 蔬菜 含量测定 

分 类 号：O657.63[理学—分析化学]