分析测试学报2024，Vol.43Issue(5)：682-689,8.DOI:10.12452/j.fxcsxb.24010203
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
Determination of Benzodiazepines in Human Urine Sample by HPLC-MS/MS Combined with ZIF-8 Based Effervescent Tablet-assisted Dispersive Solid-phase Extraction
摘要
Abstract
In this study,zeolitic imidazolate framework-8(ZIF-8)based on effervescent tablet-as-sisted dispersive solid-phase extraction method(ET-DSPE)was developed and coupled with high per-formance 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 sur-face area and pore analyzer,and the results showed that ZIF-8 nanoparticles with rhombohedral do-decahedral structure were successfully synthesized.The extraction parameters of the adsorption and elution processes were optimized in detail,involving amount of ZIF-8 sorbent and Na2CO3,adsorp-tion 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;Na2CO3 amount,20 mg;adsorption time,4 min;pH and ionic strength of the solution,no adjustment;urine dilu-tion 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(r≥0.999).The limits of detection(S/N=3)and the lim-its of quantification(S/N=10)of five BZDs were in the ranges of 0.0003-0.0006 ng/mL and 0.001-0.002 ng/mL,respectively.Besides,the recoveries for spiked urine samples with three concentra-tion levels varied from 81.6%to 108%with the intra-day relative standard deviations(RSDs)and in-ter-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 ac-curate,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Key words
urine/benzodiazepines/effervescent tablet-assisted dispersive solid-phase extraction/high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)分类
化学化工引用本文复制引用
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(5):682-689,8.基金项目
国家自然科学基金资助项目(82073608) （82073608）
河北省自然科学基金资助项目(H2022209025) （H2022209025）
华北理工大学公共卫生学院高水平科研创新团队建设计划(KYTD202302) （KYTD202302）
