β-蒎烯键合硅胶色谱固定相的制备及应用  

Preparation and Application of β-Pinene Bonded Silica Stationary Phase

作　　者：谢文博 连丽丽 曾磊 李浩 张睿哲 蒋艳忠[1] 张立颖[1] 雷福厚 XIE Wen-bo;LIAN Li-li;ZENG Lei;LI Hao;ZHANG Rui-zhe;JIANG Yan-zhong;ZHANG Li-ying;LEI Fu-hou(School of Chemical Engineering Technology,Guangxi Vocational&Technical Institute of Industry,Nanning 530001,China;Key Laboratory of Chemistry and Engineering of Forest Products of State Ethnic Affairs Commission,Guangxi Key Laboratory of Chemistry and Engineering of Forest Products,Guangxi Collaborative Innovation Center for Chemistry and Engineering of Forest Products,School of Chemistry and Chemical Engineering,Guangxi Minzu University,Nanning 530006,China)

机构地区：[1]广西工业职业技术学院化工技术学院,广西南宁530001 [2]广西民族大学化学化工学院,林产化学与工程国家民委重点实验室,广西林产化学与工程重点实验室/协同创新中心,广西南宁530006

出　　处：《分析测试学报》2025年第2期310-317,共8页Journal of Instrumental Analysis

基　　金：国家自然科学基金项目(32060325);广西自然科学基金面上项目(2023GXNSFAA026481);桂工业院科研资助(Y2020KY008)。

摘　　要：该文以β-蒎烯(β-P)为单体,通过“巯基-烯”点击化学反应将其键合到烷基化硅胶表面,制备出β-P@SiO_(2)固定相。傅里叶变换红外光谱、热重分析、比表面积及微孔物理吸附等表征结果表明,β-P@SiO_(2)固定相制备成功。色谱性能评价显示,该色谱柱具有典型的反相色谱行为和疏水选择性,以及良好的稳定性、重现性和立体选择性。采用β-P@SiO_(2)柱测得三七中5种皂苷(三七皂苷R1、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1和人参皂苷Rd)的加标回收率为94.7%~106%,粗提物中R1的含量为4.84%、Rg1为18.69%、Re为2.52%、Rb1为19.75%、Rd为5.00%。在相同的色谱条件下,β-P@SiO_(2)柱对5种皂苷的分离效果优于C18柱。采用β-P@SiO_(2)柱测得吴茱萸中吴茱萸碱和吴茱萸次碱的加标回收率为93.1%~104%,粗提物中吴茱萸碱的含量为0.086%,吴茱萸次碱的含量为0.075%,在均具有较好分离效果的条件下,C_(18)柱存在分析时间长、效率低的问题。以上结果表明该色谱柱可用于三七和吴茱萸粗提物中关键组分的分析。In this study,β-pinene(β-P)was used as functional monomer to prepare the β-P@SiO_(2) stationary phase,through the“thiol-ene”click chemical reaction.The characterization results of Fourier transform infrared spectroscopy,thermogravimetric analysis,and nitrogen adsorp⁃tion-desorption measurements showed that the β-P@SiO_(2) stationary phase was successfully prepared.In addition,chromatographic performance evaluation showed that the column exhibited typical re⁃versed-phase chromatography performance,hydrophobic selectivity,good stability,reproducibility,and steric selectivity.The LOD(S/N=3)and LOQ(S/N=10)of the five saponins in Panax notoginseng(notoginsenoside R1(R1),ginsenoside Rg1(Rg1),ginsenoside Re(Re),ginsenoside Rb1(Rb1)and ginsenoside Rd(Rd))were determined from the standard samples with the lowest concentrations,which were 22.39μg·mL^(-1) and 74.62μg·mL^(-1) for R1,20.98μg·mL^(-1) and 69.93μg·mL^(-1) for Rg1,22.98μg·mL^(-1) and 76.62μg·mL^(-1) for Re,2.76μg·mL^(-1) and 9.21μg·mL^(-1) for Rb1,and 2.4μg·mL^(-1) and 7.97μg·mL^(-1) for Rd.The recovery of standard addition of five saponins detected was 94.7%-106%.In the crude extract of Panax notoginseng,the content of R1 was 4.84%,Rg1 was 18.69%,Re was 2.52%,Rb1 was 19.75%and Rd was 5.00%.The peaks of Rg1 and Re over⁃lapped completely on the C18 column under the same chromatographic conditions,the separation effect of the five saponins on the β-P@SiO_(2) column was better than that on the C_(18) column.The LOD and LOQ of the evodiamine(EVO)and rutecarpine(RUT)in Evodiae were determined from the stan⁃dard samples with the lowest concentrations,which were 0.0983μg·mL^(-1)and 0.327μg·mL^(-1) for EVO,0.138μg·mL^(-1) and 0.46μg·mL^(-1) for RUT.The recovery of standard addition of EVO and RUT detected was 93.1%-104%.The content of EVO and RUT in the crude extract was 0.086% and 0.075%,respectively.When the separation effect was good,the analysis time of C18 column was long and the efficiency was low.The results indicated t

关 键 词：Β-蒎烯 固定相 三七 吴茱萸 

分 类 号：O657.7[理学—分析化学] R284[理学—化学]