HPLC-MS/MS法快速测定淀粉生物粘附材料特异性结合糖类物质的含量  

Rapid Detection of Glucide Specifically Linking with Starch Bioadhesive Materials by HPLC-MS/MS

作　　者：向弘[1] 朱斌[1] 王雪毓[2] 刘早[2] 李晓玺[2] 徐昕荣[1] 陈玲[2] 

机构地区：[1]华南理工大学分析测试中心,广东广州510640 [2]华南理工大学轻工与食品学院,广东广州510640

出　　处：《质谱学报》2010年第5期291-296,共6页Journal of Chinese Mass Spectrometry Society

基　　金：国家自然科学基金项目(20606014);国家支撑项目(2006BAD27B04)资助

摘　　要：研究了高效液相色谱-串联质谱（HPLC-MS/MS）法测定淀粉生物粘附材料与糖残基特异性结合实验中,岩藻糖、半乳糖、α-甲基甘露糖苷和N-乙酰葡萄糖胺4种糖类物质含量的分析方法。将反应后的样品直接离心过滤后即可利用HPLC-MS/MS进行定性定量分析。以V（乙腈）∶V（水）=80∶20的溶液作为液相色谱流动相,质谱采用电喷雾负离子电离方式扫描,以多反应监测（MRM）模式进行定量分析。在添加水平为1.0~40.0 mg.L-1范围内,岩藻糖的回收率为111.0%,相对标准偏差（RSD）为6.55%;在添加水平为1.0~80.0 mg.L-1范围内,半乳糖、α-甲基甘露糖苷和N-乙酰葡萄糖胺的回收率分别为106.5%、99.0%和91.0%,相对标准偏差分别为7.78%、6.64%和5.68%。4种糖类物质的方法检出限（S/N≥3）分别为0.1mg.L-1（岩藻糖）,1.0 mg.L-1（半乳糖）,0.1 mg.L-1（α-甲基甘露糖苷）和0.5 mg.L-1（N-乙酰葡萄糖胺）。该方法可用于评价淀粉粘附材料和糖类物质的特异性结合,为其他领域中糖类物质含量的测定提供可借鉴的方法。A method was developed in determining 4 kinds of glucides which were fucose,galactose,α-methyl mannoside and N-acetylglucosamine,in experiment of adhesive property between starch bioadhesive materials and sugar residues by high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）.The sample was filtrated and analyzed by HPLC-MS/MS.Analyte was separated by liquid chromatography with a mobile phase consisting of V（acetonitrile）∶V（water）=80∶20.The mass spectrometer was operated at the negative ion mode via electrospray ionization（ESI） source.The quantitative analysis was determined by the multiple reactions monitoring（MRM）.Linear relationship between values of peak area of detection signals and concentration of fucose are obtained in the ranges of 1.0—40.0 mg·L-1,while relationships of galactose,α-methyl mannoside and N-acetylglucosamine are obtained in the range of the linear ranges 1.0—80.0 mg·L-1.The recovery rate of fucose is 111%,and the RSD is 6.55%.The recoveries rates of galactose,α-methyl mannoside and N-acetylglucosamine are 106.5%,99.0% and 91.0%,the RSDs are 7.78%,6.64% and 5.68%,respectively.Limits of detection（S/N≥3） for fucose,galactose,α-methyl mannoside and N-acetylglucosamine are 0.1,1.0,0.1 and 0.5 mg·L-1,respectively.The method is proved to be rapid,reliable and sensitive,which is suitable for estimating the specific linking between starch bioadhesive materials and glucides.The proposed method is also suitable for rapid determination of glucides components in other complex system.

关 键 词：淀粉生物粘附材料 高效液相色谱-串联质谱(HPLC-MS/MS) 糖类物质 

分 类 号：O657.63[理学—分析化学]