色谱

色谱 ›› 2019, Vol. 37 ›› Issue (12): 1343-1348.DOI: 10.3724/SP.J.1123.2019.08004

• 研究论文 • 上一篇    下一篇

聚[2-(丙烯酰氧基)乙基]三甲基氯化铵-乙二醇二甲基丙烯酸酯整体柱固相萃取结合高效液相色谱法测定尿液中3种苯二氮（卄卓）类药物

杜梨1, 李娜1, 刘美琨1, 王翰云1, 张倩影2, 王曼曼1, 王学生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:2019-08-03 出版日期:2019-12-08 发布日期:2020-12-11
  • 通讯作者: 王曼曼.E-mail:mmwangheuu@126.com;王学生.E-mail:xswang64@163.com.
  • 基金资助:
    河北省自然科学基金项目（H2017209232）；河北省教育厅重点项目（ZD2018014）.

Determination of three benzodiazepines in human urine by solid-phase extraction with poly [2-(acryloyloxy) ethyl] trimethyl ammonium chloride-co-ethylene glycol dimethacrylate monolithic column coupled with high performance liquid chromatography

DU Li1, LI Na1, LIU Meikun1, WANG Hanyun1, ZHANG Qianying2, WANG Manman1, WANG Xuesheng1   

  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:2019-08-03 Online:2019-12-08 Published:2020-12-11
  • Supported by:
    Natural Science Foundation of Hebei Province (No. H2017209232); Research Foundation of Education Bureau of Hebei Province (No. ZD2018014).

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摘要： 以[2-（丙烯酰氧基）乙基]三甲基氯化铵（DAC）为单体，乙二醇二甲基丙烯酸酯（EDMA）为交联剂在注射器中制备聚合物整体柱，用其固相萃取尿液中溴西泮（BRZ）、劳拉西泮（LRZ）和地西泮（DZP）3种苯二氮（卄卓）类药物（BZDs），并采用高效液相色谱法（HPLC）分析。实验考察了整体柱聚合时间及固相萃取条件（淋洗溶液、洗脱溶剂种类和体积）对BZDs萃取效率的影响。结果表明，仅聚合4 h得到的整体柱对BZDs吸附效率为100%。取尿液样品4 mL上样，用4 mL H2O冲洗，1 mL乙酸乙酯洗脱，采用高效液相色谱分析。在最优条件下，3种BZDs在4.0~1000 ng/mL范围内线性关系良好（r=0.999），检出限（S/N=3）和定量限（S/N=10）分别为1.0~1.2 ng/mL和3.3~4.0 ng/mL；在10、25和50 ng/mL加标水平下回收率为81.4%~102%，日内（n=3）和日间（n=3）相对标准偏差分别为1.2%~4.5%和2.5%~8.3%。该整体柱可对尿液中3种BZDs有效净化，且富集达12~15倍。方法构筑的聚合物整体柱制备简单，萃取高效，可成功用于尿液中3种BZDs的分析。

关键词: 高效液相色谱, 固相萃取, 聚合物整体柱, [2-(丙烯酰氧基)乙基]三甲基氯化铵, 苯二氮类药物, 尿液

Abstract: A polymer monolithic column was prepared in a syringe by using [2-(acryloyloxy) ethyl] trimethyl ammonium chloride (DAC) as a monomer and ethylene glycol dimethacrylate (EDMA) as a crosslinker. The obtained monolith was developed as a solid-phase extraction sorbent and used with high performance liquid chromatography (HPLC) for the analysis of three benzodiazepines (BZDs) including bromazepam (BRZ), lorazepam (LRZ) and diazepam (DZP) in urine. The effects of reaction time and the solid-phase extraction conditions (washing solution, elution solvent and volume) on the extraction efficiencies of the three BZDs were investigated. The monolithic column was successfully prepared within 4 h, and it offered 100% adsorption efficiency for the three BZDs. The urine sample (4 mL) was loaded on the monolith, washed with 4 mL of H2O, and eluted with 1 mL of ethyl acetate. Under the optimized conditions, the linear ranges were 4.0-1000 ng/mL for the three BZDs, with correlation coefficients (r) of 0.999. The limits of detection (S/N=3) and limits of quantification (S/N=10) of the three BZDs were in the range of 1.0-1.2 ng/mL and 3.3-4.0 ng/mL, respectively. The recoveries at three spiked levels (10, 25 and 50 ng/mL) of the three BZDs ranged from 81.4% to 102%, with intra-day and inter-day relative standard deviations (n=3) of 1.2%-4.5% and 2.5%-8.3%. The polymer monolithic column provided effective purification for the three BZDs in urine and the enrichment factor was 12-15. This polymer monolithic adsorbent has the advantages of easy preparation and high extraction efficiency. It is successfully applied to the determination of the three BZDs in urine samples.

Key words: high performance liquid chromatography (HPLC), solid-phase extraction (SPE), polymeric monolithic column, [2-(acryloyloxy) ethyl] trimethyl ammonium chloride (DAC), benzodiazepines (BZDs), urine

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