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Imprinted functionalized silica sol-gel for solid-phase extraction of triazolamin
Authors:Jin Guoyou  Zhang Baofei  Tang Youwen  Zuo Xiongjun  Wang Songcai  Tang Jingyi
Affiliation:a School of Chemistry and Environment, South China Normal University, Guangzhou 510006, China
b Guangzhou Baiyunshan Pharmaceutical Co., Ltd., Guangzhou Baiyunshan Chemical Pharmaceutical Factory, Guangzhou 510515, China
c Guangzhou Forensic Science Institute, Guangzhou 510030, China
Abstract:A triazolam-imprinted silica microsphere was prepared by combining a surface molecular-imprinting technique with the sol-gel process. The results illustrate that the triazolam-imprinted silica microspheres provided using γ-aminopropyltriethoxysilane and phenyltrimethoxysilane as monomers exhibited higher selectivity than those provided from γ-aminopropyltriethoxysilane and methyltriethoxysilane. In addition, the optimum affinity occurred when the molar ratio of γ-aminopropyltriethoxysilane, phenyltrimethoxysilane, and the template molecule was 4.2:4.7:0.6. Retention factor (k) and imprinting factor (IF) of triazolam on the imprinted and non-imprinted silica microsphere columns were characterized using high performance liquid chromatography (HPLC) with different mobile phases including methanol, acetonitrile, and water solutions. The molecular selectivity of the imprinted silica microspheres was also evaluated for triazolam and its analogue compounds in various mobile phases. The better results indicated that k and IF of triazolam on the imprinted silica microsphere column were 2.1 and 35, respectively, when using methanol/water (1/1, v/v) as the mobile phase. Finally, the imprinted silica was applied as a sorbent in solid-phase extraction (SPE), to selectively extract triazolam and its metabolite, α-hydroxytriazolam, from human urine samples. The limits of detection (LOD) for triazolam and α-hydroxytriazolam in urine samples were 30 ± 0.21 ng mL−1 and 33 ± 0.26 ng mL−1, respectively.
Keywords:Surface imprinting   Solid-phase extraction   Triazolam   Metabolite   Urine sample
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