Determination of 12 Benzodiazepines Drugs in Urine Using Polydimethylsiloxane Sponge-assisted Dispersive Liquid-Liquid Microextraction Coupled with GC-MS

LIANG Wei-wei; LIU Yue; LIN Xian-wen; ZHU Huan-hui; SUN Li-min; CHEN Xiao-hui; WANG Song-cai

doi:10.12452/j.fxcsxb.240708202

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Determination of 12 Benzodiazepines Drugs in Urine Using Polydimethylsiloxane Sponge-assisted Dispersive Liquid-Liquid Microextraction Coupled with GC-MS

Scientific Papers | 更新时间：2025-03-17

- Determination of 12 Benzodiazepines Drugs in Urine Using Polydimethylsiloxane Sponge-assisted Dispersive Liquid-Liquid Microextraction Coupled with GC-MS
- Journal of Instrumental Analysis Vol. 44, Issue 3, Pages: 464-470(2025)
- 作者机构：
  
  广州市刑事科学技术研究所，广东广州 510000
- 作者简介：
- 基金信息：
- DOI：10.12452/j.fxcsxb.240708202
  CLC： O657.1;S859.81
- Received：08 July 2024，
  
  Revised：27 August 2024，
  
  Accepted：2024-09-04，
  
  Published：15 March 2025
- 稿件说明：
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梁未未,刘悦,林贤文,朱焕慧,孙立敏,陈晓晖,王松才.尿液中12种苯二氮卓类药物的聚二甲基硅氧烷海绵辅助分散液液微萃取/GC-MS法检测[J].分析测试学报,2025,44(03):464-470.

LIANG Wei-wei,LIU Yue,LIN Xian-wen,ZHU Huan-hui,SUN Li-min,CHEN Xiao-hui,WANG Song-cai.Determination of 12 Benzodiazepines Drugs in Urine Using Polydimethylsiloxane Sponge-assisted Dispersive Liquid-Liquid Microextraction Coupled with GC-MS[J].Journal of Instrumental Analysis,2025,44(03):464-470.
梁未未,刘悦,林贤文,朱焕慧,孙立敏,陈晓晖,王松才.尿液中12种苯二氮卓类药物的聚二甲基硅氧烷海绵辅助分散液液微萃取/GC-MS法检测[J].分析测试学报,2025,44(03):464-470. DOI： 10.12452/j.fxcsxb.240708202.

LIANG Wei-wei,LIU Yue,LIN Xian-wen,ZHU Huan-hui,SUN Li-min,CHEN Xiao-hui,WANG Song-cai.Determination of 12 Benzodiazepines Drugs in Urine Using Polydimethylsiloxane Sponge-assisted Dispersive Liquid-Liquid Microextraction Coupled with GC-MS[J].Journal of Instrumental Analysis,2025,44(03):464-470. DOI： 10.12452/j.fxcsxb.240708202.

摘要

设计了一种基于疏水多孔聚二甲基硅氧烷海绵辅助的分散液液微萃取装置（PDMS-Sponge-DLLME），并实现了对尿液中12种常见苯二氮卓类（BZDs）安眠药的快速高效提取，借助气相色谱-质谱（GC-MS）直接进样完成检验鉴定。通过方糖提供的骨架实现疏水多孔有机PDMS海绵材料的制备，采用傅里叶变换红外光谱、扫描电镜对其微观结构性能进行表征，结合医用注射器、磁搅拌子及橡胶堵头完成该萃取装置的组装，利用内标法进行定量分析。在最优条件下，尿液中12种常见安眠药在0.1~10 µg/mL范围内具有良好的线性关系，相关系数（

）均大于0.99，检出限为0.025~0.200 µg/mL，定量下限为0.050~0.400 µg/mL，3个加标水平下的回收率为64.4%~112%，相对标准偏差为0.80%~9.4%。该新型分散液液微萃取装置可在数分钟内完成对尿液中安眠药的高效提取、富集，借助GC-MS即可实现快速检验，具有绿色、高效、简便、廉价等优势。

Abstract

A dispersive liquid-liquid microextraction（DLLME） device based on hydrophobic porous polydimethylsiloxane sponge（PDMS-Sponge） was established to achieve rapid and efficient extraction of 12 common benzodiazepines drugs in urine. Direct injection test and identification method were achieved with the assistance of gas chromatography-mass spectrometry（GC-MS）. The preparation of hydrophobic p

orous organic PDMS sponge material was achieved through the framework provided by sugar cubes. Fourier transforminfrared spectrometer and scanning electron microscopy were used to characterize the microstructure and performance of PDMS-Sponge. The extraction device was completed by combining medical syringes，magnetic stirrers，and rubber plugs. Quantitative analysis using the internal standard method was conducted to investigate the effects of dispersant，pH value，magnetic stirring time，and dispersant dosage on the extraction efficiency of 12 drugs in urine. The results showed that PDMS-Sponge is a hydrophobic porous material，which can be combined with a medical syringe to construct a new dispersive liquid-liquid microextraction device. Using 100 µL of dichloromethane as the extractant，50 µL of acetonitrile as the dispersant，a speed of 800 r/min，and magnetic stirring for 1 min can achieve the extraction and enrichment of the analytes. Under optimal conditions，12 common hypnotics in urine have a good linear relationship in the range of 0.1-10 µg/mL，with correlation coefficients（

） greater than 0.99，detection limits of 0.025-0.200 µg/mL，and quantitation limits of 0.050-0.400 µg/mL. The recoveries at three spiked levels was 64.4%-112%，and the relative standard deviations was 0.80%-9.4%. The newly dispersive liquid-liquid microextraction device can complete the efficient extraction and concentration of hypnotics in urine in a few minutes，and rapid testing can be achieved with the assistance of GC-MS，providing a green，efficient，simple and inexpensive new dispersive liquid-liquid microextraction solution.

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