亲水性相互作用色谱-四极杆串联线性离子阱质谱测定蛋白食品中L-羟脯氨酸残留  

Determination of L-Hydroxyproline by Hydrophilic Interaction Chromatography Coupled Tandem Quadrupole Linear Ion Trap Mass Spectrometry in Protein Contained Food

作　　者：赵善贞[1] 邓晓军[1] 彭涛[2] 伊雄海[1] 郭德华[1] 韩丽[1] 盛永刚[1] 吴巧彬[3] 

机构地区：[1]上海出入境检验检疫局,上海200135 [2]中国检验检疫科学研究院,北京100025 [3]上海海洋大学,上海200433

出　　处：《分析化学》2011年第9期1373-1379,共7页Chinese Journal of Analytical Chemistry

基　　金：上海市科委技术标准专项(No.09DZ0503700);长三角科技合作项目(No.10595812100);质检公益性行业专项(No.201010073-04);国家质检总局课题(No.2009IK314;2011IK232)资助

摘　　要：建立了亲水性相互作用色谱-四极杆串联线性离子阱质谱检测含蛋白食品中的皮革水解蛋白标示物L-羟脯氨酸(L-HYP)的同时定性与定量分析方法。样品中的L-HYP经酶解后用乙腈沉淀蛋白,HLB小柱除去部分脂溶性干扰物,采用液相色谱-质谱进行测定。本方法采用IDA结合EPI模式对试样中的L-HYP进行定性分析,并建立L-HYP的二级子离子谱库。通过以MRM模式对L-HYP进行定量分析,L-HYP在12种蛋白食品中平均回收率在73.4%～114.2%(n=6)之间,相对标准偏差在2.5%～14.4%(n=6)之间,可对试样中的L-HYP在定性确证的同时进行定量分析。A method based on hydrophilic interaction chromatography-quadrupole/linear ion trap-mass spectrometry（HILIC-q/LTQ MS） for qualitative and quantitative determination of L-hydroxyproline（L-HYP） as target compound in protein contained-food was presented.L-hydroxyproline in samples were extracted with acetonitrile after enzymolysis,followed by a further cleanup using HLB solid phase extraction column to remove lipid soluble interferes.The L-HYP residue was separated upon a hydrophilic interaction chromatography column and determined by quadrupole-linear ion trap-mass spectrometry.Information dependent acquisition scan function（IDA） combined with enhanced product ion scan（EPI） library was used to confirm the content of L-HYP,while quantification was operated by MRM mode.The recoveries ranged from 73.4% to 114.2%（n=6） and the RSD between 2.5% and 14.4%（n=6） in 12 kinds of protein contained matrices respectively.

关 键 词：L-羟脯氨酸 亲水性相互作用色谱 四极杆串联线性离子阱质谱 皮革水解蛋白 

分 类 号：TS207.3[轻工技术与工程—食品科学] O657.63[轻工技术与工程—食品科学与工程]