分析测试学报2025，Vol.44Issue(3)：464-470,7.DOI:10.12452/j.fxcsxb.240708202
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
Determination of 12 Benzodiazepines Drugs in Urine Using Polydimethylsiloxane Sponge-assisted Dispersive Liquid-Liquid Microextraction Coupled with GC-MS
摘要
Abstract
A dispersive liquid-liquid microextraction(DLLME)device based on hydrophobic porous polydimethylsiloxane sponge(PDMS-Sponge)was established to achieve rapid and efficient extrac-tion 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 prepara-tion of hydrophobic porous organic PDMS sponge material was achieved through the framework provid-ed 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 analy-sis using the internal standard method was conducted to investigate the effects of dispersant,pH val-ue,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.Un-der optimal conditions,12 common hypnotics in urine have a good linear relationship in the range of 0.1-10 µg/mL,with correlation coefficients(r2)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 liq-uid-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,provid-ing a green,efficient,simple and inexpensive new dispersive liquid-liquid microextraction solution.关键词
聚二甲基硅氧烷海绵/分散液液微萃取/苯二氮卓类药物/尿液/气相色谱-质谱Key words
polydimethylsiloxane sponge/dispersive liquid-liquid microextraction/benzodiaze-pines/urine/gas chromatography-mass spectrometry分类
化学引用本文复制引用
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(3):464-470,7.基金项目
广州市民生科技攻关专题(2019030009) （2019030009）
