title: Determination of propofol glucuronide from hair sample by using mixed mode anion exchange cartridge and liquid chromatography tandem mass spectrometry.
abstract: The main objective of this study was to develop and validate a simpler and less time consuming analytical method for determination of propofol glucuronide from hair sample, by using mixed mode anion exchange cartridge and liquid chromatography-tandem mass spectrometry (LC-MS/MS). The study uses propofol glucuronide, a major metabolite of propofol, as a marker for propofol abuse. The hair sample was digested in sodium hydroxide solution and loaded in mixed-mode anion cartridge for solid phase extraction. Water and ethyl acetate were used as washing solvents to remove interfering substances from the hair sample. Consequently, 2% formic acid in ethyl acetate was employed to elute propofol glucuronide from the sorbent of mixed-mode anion cartridge, and analyzed by LC-MS/MS. The method validation parameters such as selectivity, specificity, LOD, LLOQ, accuracy, precision, recovery, and matrix effect were also tested. The linearity of calibration curves showed good correlation, with correlation coefficient 0.998. The LOD and LLOQ of the propofol glucuronide were 0.2 pg/mg and 0.5 pg/mg, respectively. The intra and inter-day precision and accuracy were acceptable within 15%. The mean values of recovery and matrix effect were in the range of 91.7-98.7% and 87.5-90.3%, respectively, signifying that the sample preparation, washing and extraction procedure were efficient, and there was low significant hair matrix effect for the extraction of propofol glucuronide from hair sample on the mixed mode anion cartridge. To evaluate the suitability of method, the hair of propofol administered rat was successfully analyzed with this method.
authors.affiliation: College of Pharmacy, Kyungsung University, Busan 608-736, Republic of Korea.
authors.forename: Jae-Hwan
authors.initials: JH
authors.lastname: Kwak
authors.affiliation: College of Pharmacy, Kyungsung University, Busan 608-736, Republic of Korea.
authors.forename: Hye Kyung
authors.initials: HK
authors.lastname: Kim
authors.affiliation: Drug and Toxicology Section, Busan Institute, National Forensic Service, Yangsan 626-815, Republic of Korea.
authors.forename: Sanggil
authors.initials: S
authors.lastname: Choe
authors.affiliation: Drug & Forensic Toxicology Division, National Forensic Service, 10 Ipchunro, Wonjusi, Gangwondo 26460, Republic of Korea.
authors.forename: Sangwhan
authors.initials: S
authors.lastname: In
authors.affiliation: College of Pharmacy, Kyungsung University, Busan 608-736, Republic of Korea. Electronic address: jspyo@ks.ac.kr.
authors.forename: Jae Sung
authors.initials: JS
authors.lastname: Pyo
mesh_terms: D000818:Animals; D002852:Chromatography, Ion Exchange / Q000379:methods*; D020719:Glucuronides / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D006197:Hair / Q000737:chemistry*; D057230:Limit of Detection; D016014:Linear Models; D008297:Male; D015742:Propofol / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D051381:Rats; D015203:Reproducibility of Results; D052616:Solid Phase Extraction; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D020719:Glucuronides; D015742:Propofol
keywords: Hair analysis; LC–MS/MS; Propofol glucuronide; Solid phase extraction