Determination of Benzodiazepines in Human Urine Sample by HPLC-MS/MS Combined with ZIF-8 Based Effervescent Tablet-assisted Dispersive Solid-phase Extraction

ZHAO Zhi-dong; XIA Lei; ZHAO Jun-jian; CUI Chuan-jin; FENG Cheng-ling; WANG Man-man

doi:10.12452/j.fxcsxb.24010203

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Determination of Benzodiazepines in Human Urine Sample by HPLC-MS/MS Combined with ZIF-8 Based Effervescent Tablet-assisted Dispersive Solid-phase Extraction

Scientific Papers | 更新时间：2024-08-16

- Determination of Benzodiazepines in Human Urine Sample by HPLC-MS/MS Combined with ZIF-8 Based Effervescent Tablet-assisted Dispersive Solid-phase Extraction
- Journal of Instrumental Analysis Vol. 43, Issue 5, Pages: 682-689(2024)
- 作者机构：
  
  1.华北理工大学公共卫生学院，河北唐山 063210
  2.华北理工大学电气工程学院，河北唐山 063210
  3.华北理工大学附属医院，河北唐山 063000
- 作者简介：
- 基金信息：
- DOI：10.12452/j.fxcsxb.24010203
  CLC： O657.7;R113
- Published：15 May 2024，
  
  Received：02 January 2024，
  
  Revised：29 January 2024，
- 稿件说明：
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赵志栋,夏磊,赵俊暕,崔传金,封成玲,王曼曼.ZIF-8泡腾辅助分散固相萃取结合高效液相色谱-串联质谱法测定人尿液中苯二氮卓类药物[J].分析测试学报,2024,43(05):682-689.

ZHAO Zhi-dong,XIA Lei,ZHAO Jun-jian,CUI Chuan-jin,FENG Cheng-ling,WANG Man-man.Determination of Benzodiazepines in Human Urine Sample by HPLC-MS/MS Combined with ZIF-8 Based Effervescent Tablet-assisted Dispersive Solid-phase Extraction[J].Journal of Instrumental Analysis,2024,43(05):682-689.
赵志栋,夏磊,赵俊暕,崔传金,封成玲,王曼曼.ZIF-8泡腾辅助分散固相萃取结合高效液相色谱-串联质谱法测定人尿液中苯二氮卓类药物[J].分析测试学报,2024,43(05):682-689. DOI： 10.12452/j.fxcsxb.24010203.

ZHAO Zhi-dong,XIA Lei,ZHAO Jun-jian,CUI Chuan-jin,FENG Cheng-ling,WANG Man-man.Determination of Benzodiazepines in Human Urine Sample by HPLC-MS/MS Combined with ZIF-8 Based Effervescent Tablet-assisted Dispersive Solid-phase Extraction[J].Journal of Instrumental Analysis,2024,43(05):682-689. DOI： 10.12452/j.fxcsxb.24010203.

摘要

发展了基于沸石咪唑酯骨架材料-8（ZIF-8）的泡腾辅助分散固相萃取（ET-DSPE）技术，结合高效液相色谱-串联质谱法（HPLC-MS/MS）对人

尿液中艾司唑仑、阿普唑仑、地西泮、三唑仑和劳拉西泮5种苯二氮卓类药物（BZDs）进行分析。采用傅里叶变换红外光谱、X射线衍射仪、扫描电子显微镜和全自动比表面积及孔隙分析仪对ZIF-8进行表征，并考察了ZIF-8和Na

用量、吸附时间、溶液pH值及离子强度、尿液稀释比例、洗脱溶剂、洗脱体积和时间对BZDs萃取效率的影响。在最佳条件下，艾司唑仑在0.002~100 ng/mL，其余4种BZDs在0.001~100 ng/mL范围内线性关系良好（

≥0.999），检出限和定量下限分别为0.000 3~0.000 6 ng/mL和0.001~0.002 ng/mL，3个加标水平下的回收率为81.6%~108%，日内和日间相对标准偏差分别为1.4%~5.6%和1.4%~9.9%。该方法不仅能够直接处理原始尿液，无需稀释和去蛋白操作，而且通过泡腾辅助分散，对BZDs的富集倍数达40.8~54.0倍，实现了尿液中5种BZDs的准确、简便和灵敏分析。

Abstract

In this study，zeolitic imidazolate framework-8（ZIF-8） based on effervescent tablet-assisted dispersive solid-phase extraction method（ET-DSPE） was developed and coupled with high performance liquid chromatography tandem mass spectrometry（HPLC-MS/MS） for the determination of five benzodiazepines（BZDs） in human urine samples，including estazolam，alprazolam，diazepam，triazolam and lorazepam. The prepared ZIF-8 sorbent was characterized by Fourier transform infrared spectroscopy，X-ray powder diffractometry，scanning electron microscopy，automatic specific surface area and pore analyzer，and the results showed that ZIF-8 nanoparticles with rhombohedral dodecahedral structure were successfully synthesized. The extraction parameters of the adsorption and elution processes were optimized in detail，involving amount of ZIF-8 sorbent and Na

，adsorption time，pH and ionic strength of solution，urine dilution ratio，elution solvent，elution volume and time. The optimal conditions were shown as follows：ZIF-8 amount，35 mg；Na

amount，20 mg；adsorption time，4 min；pH and ionic strength of the solution，no adjustment；urine dilution ratio，no dilution；elution，1.0 mL of methanol；elution time，30 min. Under the optimized conditions，the proposed method provided the linear ranges of 0.002-100 ng/mL for estazolam and 0.001-100 ng/mL for the other four analytes（

≥0.999）. The limits of detection（

=3） and the limits of quan

tification（

=10） of five BZDs were in the ranges of 0.000 3-0.000 6 ng/mL and 0.001-0.002 ng/mL，respectively. Besides，the recoveries for spiked urine samples with three concentration levels varied from 81.6% to 108% with the intra-day relative standard deviations（RSDs） and inter-day RSDs of 1.4%-5.6% and 1.4%-9.9% separately. Compared with the previous pretreatment methods for BZDs in urine samples，ZIF-8 based effervescent tablet-assisted dispersive solid-phase extraction method allowed direct loading of crude urine samples without any filtration or dilution step. Besides，the effervescent tablet-assistance facilitated a well dispersion and an adequate adsorption，offering the enhancement factor of 40.8-54.0. The developed method achieved a strategy for the accurate，convenient and sensitive determination of five BZDs in human urine samples.

关键词

尿液苯二氮卓类药物泡腾辅助分散固相萃取高效液相色谱-串联质谱法

Keywords

urinebenzodiazepineseffervescent tablet-assisted dispersive solid-phase extractionhigh performance liquid chromatography tandem mass spectrometry（HPLC-MS/MS）

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