Microchimica Acta

, 186:125 | Cite as

One-pot synthesis of SiO2@SiO2 core-shell microspheres with controllable mesopore size as a new stationary phase for fast HPLC separation of alkyl benzenes and β-agonists

  • Hongjun Xia
  • Jun Wang
  • Gang Chen
  • Jiawei LiuEmail author
  • Guangpin Wan
  • Quan BaiEmail author
Original Paper


Monodisperse SiO2@SiO2 core-shell silica microspheres (CSSM) with enlarged mesopores perpendicular to the particles surface were prepared using a dual-templating approach. With cetyltrimethyl ammonium bromide as the template and octyltrimethyl ammonium bromide as an auxiliary chemical, the pore size can be enlarged from 2.6 to 10.6 nm. The average shell thickness can be increased from 31 nm to 97 nm by adjusting the concentrations of the surfactants under continuous addition of tetraethyl orthosilicate. After coating twice, the resulting CSSM has a uniform mesoporous shell of about 198 nm thickness and a narrow pore size distribution. The CSSM were then modified with octadecyltrichlorosilane to give a material referred to as CS-C18. It was evaluated by separating the mixture of methylbenzene (toluene), ethylbenzene, n-propylbenzene, n-butylbenzene, n-amylbenzene and hexylbenzene. The baseline separation of the six alkyl benzenes is achieved within 2 min. Compared to a commercial column of type BEH-C18, CS-C18 shows a faster and better separation even at lower back pressure. It was also applied to the fast separation of benzo[a]pyrene, salbutamol, ractopamine and clenbuterolin residues in pork samples. The high column efficiency and better reproducibility suggest that the CSSM can be used as a matrix for fast separation and analysis of several kinds of small analytes.

Graphical abstract

A dual-templating approach was utilized to produce the core shell microsphere with controllable mesopore channels by using hexadecyltrimethylammonium bromide (CTAB) as the template and trioctylmethylammonium bromide (TOMAB) as an auxiliary chemical to enlarge the size of CTAB micelles.


Monodisperse silica microsphere Mesoporous material Radially oriented channel Stationary phase Alkyl benzene homologues β-agonists HPLC 



This work is supported by the National Nature Science Foundation of China (21874106, 21545007, 21605122), Shaanxi Provincial Science and Technology Coordinating Innovation Projects (2013SZS18-K01), Natural Science Foundation of Shaanxi Province (2018JZ2001, 2018JQ2011) the Foundation of Key Laboratory in Shaanxi Province (2010JS103, 11JS097, 15JS115, 16JS116) and Scientific Research Foundation of the Higher Education Institutions of Henan Province (18B150030).

Compliance with ethical standards

The author(s) declare that they have no competing interests.

Supplementary material

604_2019_3229_MOESM1_ESM.doc (13.2 mb)
ESM 1 (DOC 13.2 mb)


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Copyright information

© Springer-Verlag GmbH Austria, part of Springer Nature 2019

Authors and Affiliations

  1. 1.Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, Institute of Modern Separation Science, Key Lab of Modern Separation Science in Shaanxi ProvinceNorthwest UniversityXi’anChina
  2. 2.Henan Key Laboratory of Rare Earth Functional MaterialsZhoukou Normal UniversityZhoukouChina
  3. 3.Shaanxi Research Design Institute of Petroleum and Chemical IndustryShaanxi Dangerous Chemical Supervision and Inspection CenterXi’anChina
  4. 4.Hydrocarbon High-efficiency Utilization Technology Research CenterShaanxi Yanchang Petroleum Group Co. LtdXi’anChina

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