Citation: LI Na, CHEN Xuelei, ZHANG Lei, ZHANG Qianying, AN Zhuangzhuang, SUN Xin, WANG Manman, XU Houjun. Determination of carbamazepine and 10-hydroxy-carbamazepine in human serum by solid-phase extraction with poly ethylene glycol dimethacrylate monolithic column coupled with high performance liquid chromatography[J]. Chinese Journal of Chromatography, ;2018, 36(11): 1105-1111. doi: 10.3724/SP.J.1123.2018.07025 shu

Determination of carbamazepine and 10-hydroxy-carbamazepine in human serum by solid-phase extraction with poly ethylene glycol dimethacrylate monolithic column coupled with high performance liquid chromatography

1.
School of Public Health, North China University of Science and Technology, Tangshan 063210, China;
2.
North China University of Science and Technology Affiliated Hospital, Tangshan 063000, China

Received Date: 25 July 2018

Fund Project: National Natural Science Foundation of China (No. 21305028)

A polymeric monolithic solid phase extraction sorbent was fabricated from sole ethylene glycol dimethacrylate in a syringe and applied as a sorbent for the determination of carbamazepine (CBZ) and 10-hydroxy-carbamazepine (MHD) in human serum using high performance liquid chromatography. The effects of reaction temperature and reaction time on the extraction performance of the target compounds were investigated. The parameters, such as washing solvent, and elution solution and its volume, were optimized. Under the optimized condition, the purification and enrichment of CBZ and MHD in human serum were successfully achieved on the proposed poly ethylene glycol dimethacrylate (EDMA) monolithic column. The linear ranges were 0.02-40 μg/mL for CBZ and 0.05-100 μg/mL for MHD. The results indicated that the method exhibited good linearity in the corresponding ranges with the correlation coefficients (r) of 0.999. The limits of detection (S/N=3) of CBZ and MHD were 0.004 μg/mL and 0.01 μg/mL, respectively. The average recoveries at three spiked levels of CBZ and MHD were 92.7% and 94.2%, respectively, with relative standard deviations (RSDs) ≤ 6.1%. Furthermore, the intra column to column (n=3) and inter batch to batch (n=5) RSDs were no more than 5.3%. The RSDs of eight repeated extraction cycles were no more than 5.8%. The developed method is effective and simple, and is suitable for the determination of CBZ and MHD in human serum.
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1.
沈阳化工大学材料科学与工程学院沈阳 110142