Semi-automated filter micro-solid phase extraction based on urea-formaldehyde microsphere followed by corona discharge-ion mobility spectrometry for simultaneous detection of fentanyl and nor-fentanyl in urine

• Published in: Microchemical journal 2024-05, Vol.200, p.110213, Article 110213
• Main Authors: Sun, Tangqiang, Cheng, Huining, Chu, Xunuo, Zhu, Yuzhen, Zheng, Shibo, Wang, Mengzhen, Ren, Haolei, Yan, Huijuan, He, Xiaodan, Wang, Di, Du, Zhenxia
• Format: Article
• Language: English
• Subjects: Corona discharge ionization-ion mobility spectrometry (CD-IMS); Fentanyl-related substances; On-site; Semi-automated filter micro-solid phase extraction (SA-FμSPE)
• ISSN: 0026-265X
• DOI: 10.1016/j.microc.2024.110213

[Display omitted] •SA-FμSPE was coupled with CD-IMS for the first time.•UF sorbents were prepared through a facile strategy using low-cost chemicals.•SA-FμSPE-IMS can perform on-site screening for (nor-) fentanyl in urine.•The extraction procedure attains a high score in greenness evaluation.•The proposed method indicated satisfactory extraction and analysis performance. In this work, semi-automated filter micro-solid phase extraction (SA-FμSPE) packed by urea–formaldehyde (UF) microspheres coupled with corona discharge ionization-ion mobility spectrometry (CD-IMS) was developed for the extraction and determination of fentanyl and nor-fentanyl in urine samples. UF microspheres, synthesized by aqueous polymerization, can be used to achieve effective extraction of analytes through multiple adsorption interactions such as hydrophobic, dipole–dipole and hydrogen bonding interactions. UF microspheres dispersed in methanol were packed in the filter by syringe, and the extraction process was performed by a portable automatic filter extraction device. The parameters affecting extraction efficiency (i.e., extraction time, the flow rate of extraction, pH value, amount of sorbent, ionic strength, cycle times of desorption, and type of eluent) were investigated. Then, the eluate containing fentanyl and nor-fentanyl was simultaneously analyzed by CD-IMS in positive mode. Under the optimal extraction conditions, the detection limits for the target compounds were 5.00 ng mL−1 and 8.00 ng mL−1, respectively. The spiked recoveries were in the range of 81.97 % −112.37 % by testing the real samples and validated by UHPLC-MS. Thus, the satisfactory results reveal that SA-FμSPE coupled with CD-IMS has great potential for on-site extraction and detection of fentanyl and nor-fentanyl in urine samples.