色谱

色谱 ›› 2018, Vol. 36 ›› Issue (11): 1105-1111.DOI: 10.3724/SP.J.1123.2018.07025

• 研究论文 • 上一篇    下一篇

聚乙二醇二甲基丙烯酸酯整体柱固相萃取-高效液相色谱法测定血清中卡马西平和10-羟基卡马西平

李娜1, 陈雪蕾1, 张磊1, 张倩影2, 安壮壮1, 孙鑫1, 王曼曼1, 徐厚君1   

  1. 1. 华北理工大学公共卫生学院, 河北 唐山 063210;
    2. 华北理工大学附属医院, 河北 唐山 063000
  • 收稿日期:2018-07-25 出版日期:2018-11-08 发布日期:2014-09-30
  • 通讯作者: 王曼曼.E-mail:mmwangheuu@126.com;徐厚君.E-mail:houjunxu@126.com.
  • 基金资助:

    国家自然科学基金项目（21305028）；河北省自然科学基金项目（H2017209232，H2016209018）；河北省教育厅研究项目（ZD2018014）；华北理工大学培育基金项目（JQ201717）.

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

LI Na1, CHEN Xuelei1, ZHANG Lei1, ZHANG Qianying2, AN Zhuangzhuang1, SUN Xin1, WANG Manman1, XU Houjun1   

  1. 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:2018-07-25 Online:2018-11-08 Published:2014-09-30
  • Supported by:

    National Natural Science Foundation of China (No. 21305028); Natural Science Foundation of Hebei Province (Nos. H2017209232, H2016209018); Research Foundation of Education Bureau of Hebei Province (No. ZD2018014); Training Foundation of North China University of Science and Technology (No. JQ201717).

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摘要：

使用乙二醇二甲基丙烯酸酯（EDMA）在注射器中构筑固相萃取整体柱，并结合高效液相色谱法，建立了测定血清中卡马西平（CBZ）和10-羟基卡马西平（MHD）的分析方法。实验考察了反应温度和反应时间对整体柱萃取性能的影响和淋洗溶液种类、洗脱溶液种类及体积对固相萃取的影响。在优化条件下，该固相萃取柱对血清中CBZ和MHD能够有效富集、净化。对0.02~40 μg/mL CBZ和0.05~100 μg/mL MHD标准溶液进行分析，结果表明，在各自的范围内CBZ和MHD线性关系良好，相关系数（r）均为0.999。CBZ和MHD的检出限分别为0.004 μg/mL和0.01 μg/mL；在3个加标水平下，CBZ和MHD的平均回收率分别为92.7%和94.2%，日内（n=3）和日间（n=3） RSD≤6.1%。该固相萃取柱批内（n=3）和批间（n=5） RSD≤5.3%，反复使用8次的RSD≤5.8%。该法简单、高效，适用于癫痫患者血清中CBZ和MHD的测定。

关键词: 10-羟基卡马西平, 高效液相色谱, 固相萃取, 聚合物整体柱, 卡马西平, 血清, 乙二醇二甲基丙烯酸酯

Abstract:

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.

Key words: 10-hydroxy-carbamazepine (MHD), carbamazepine (CBZ), ethylene glycol dimethacrylate (EDMA), high performance liquid chromatography (HPLC), polymeric monolithic column, serum, solid-phase extraction (SPE)

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