"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.
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.
Meiyun
M
Xue
Hongxue
H
Huang
Yanxiong
Y
Ke
Changhu
C
Chu
Yu
Y
Jin
Xinmiao
X
Liang
D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation* / Q000379:methods; D004151:Dipeptides / Q000737:chemistry*; D012250:Rheum / Q000737:chemistry
D004151:Dipeptides