"Click dipeptide": a novel stationary phase applied in two-dimensional liquid chromatography.
2D-HPLC is an important technique for the separation of complex samples. Developing new types of stationary phases is of great interest to construct 2D-LC systems with high orthogonality. In this study, a novel stationary phase-Click dipeptide (l-phenylglycine dipeptide) was prepared by immobilization of alpha-azido l-phenylglycine dipeptide on alkyne-silica via click chemistry. In the preparation of this new material, an efficient, inexpensive and shelf-stable diazo transfer reagent (imidazole-1-sulfonyl azide hydrochloride) was utilized to transfer the amino group of l-phenylglycine to corresponding azido group under mild conditions. The Click dipeptide thus prepared was confirmed by FT-IR, solid state CP/MAS (13)C NMR and elemental analysis. The Click dipeptide packing showed high orthogonality with C18, which reached 63.5%. An off-line 2D-RP/RPLC system was developed to analyze a traditional Chinese medicine (TCM)-Rheum Palmatum L. The results showed high orthogonality between Click dipeptide and C18 as well as great separating power in the practical separation of complex samples.
Xue
Meiyun
M
Engineering Research Center of Pharmaceutical Process Chemistry, Ministry of Education, School of Pharmacy, East China University of Science and Technology, 130 Meilong Road, Shanghai, 200237, China.
Huang
Hongxue
H
Ke
Yanxiong
Y
Chu
Changhu
C
Jin
Yu
Y
Liang
Xinmiao
X
D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation* / Q000379:methods; D004151:Dipeptides / Q000737:chemistry*; D012250:Rheum / Q000737:chemistry
D004151:Dipeptides