UPLC-MS/MS测定小麦茎秆木质素单体交联结构的方法  

Determination of Lignin Monomer Crosslinking Structures in Wheat Stems by UPLC-MS/MS

作　　者：孙淑芳 骆永丽[1] 李春辉 金敏 胥倩 SUN Shu-fang;LUO Yong-li;LI Chun-hui;JIN Min;XU Qian(Agricultural College,Shandong Agricultural University/State Key Laboratory of Crop Biology,Tai'an 271018)

机构地区：[1]山东农业大学农学院作物生物学国家重点实验室,泰安271018

出　　处：《生物技术通报》2022年第10期66-72,共7页Biotechnology Bulletin

基　　金：国家自然科学基金项目(31801330,32101834,32172117);山东省自然科学基金(ZR2020QC106);山东省泰山产业领军人才计划(LJNY2015001);国家重点研发计划(2017YFD0301001,2016YFD0300403)。

摘　　要：建立一种利用UPLC-MS/MS对小麦茎秆木质素单体交联结构进行定性与定量分析的方法,为木质素的开发利用提供科学依据。采用ACQUITY UPLC®BEH C_(18)(2.1 mm×100 mm,1.7μm)色谱柱分离,以超纯水和乙腈为流动相进行梯度洗脱,选择MRM(多反应监测模式)进行检测。结果表明,9种木质素单体交联结构在相关线性范围内线性良好(R^(2)=0.9989),回收率为91.67%-100%,相对标准偏差(RSD)为0.24%-2.10%。将该方法应用于拔节后14 d小麦茎秆中9种木质素单体交联结构特性的检测,结果显示,样品中9种木质素单体交联结构的保留时间与标准品的保留时间相同,G(8-8)G是检出质量浓度最高的木质素单体交联结构,质量浓度范围为9.53-10.12 ng/g。该方法专一性强,灵敏度高,适用于对小麦茎秆9种木质素单体交联结构进行准确定性定量。A method for the qualitative and quantitative determination of lignin monomer crosslinking structures in wheat stems by UPLC-MS/MS was established,providing a scientific basis for the development and utilization of lignin.The chromatographic separation was carried out on an ACQUITY UPLC®BEH C18(2.1 mm×100 mm,1.7μm),ultrapure water and acetonitrile were used as the mobile phase to conduct gradient elution,and MRM(multiple reaction monitoring)were employed for detection.The results showed that the crosslinking structures of 9 lignin monomers had good linearity in the linear correlation range(R^(2)=0.9989),the recovery was 91.67%-100%,and the relative standard deviations was 0.24%-2.10%.The method was applied to detect the crosslinking structure characteristics of 9 lignin monomers in wheat stems 14 d after jointing.The results revealed that the retention times of the crosslinking structures of 9 lignin monomers in the sample were the same as that of the standard one.G(8-8)G was the crosslinking structure of lignin monomers with the highest mass concentration,and the mass concentration range was 9.53-10.12 ng/g.In conclusion,the method is of strong specificity and high sensitivity.It is suitable for accurate qualitative and quantitative analysis of the crosslinking structures of nine lignin monomers in the wheat stems.

关 键 词：UPLC-MS/MS 小麦 茎秆 木质素单体交联结构 回收率 

分 类 号：S512.1[农业科学—作物学]