title: Comparison of two automated solid phase extractions for the detection of ten fentanyl analogs and metabolites in human urine using liquid chromatography tandem mass spectrometry.
abstract: Two types of automated solid phase extraction (SPE) were assessed for the determination of human exposure to fentanyls in urine. High sensitivity is required to detect these compounds following exposure because of the low dose required for therapeutic effect and the rapid clearance from the body for these compounds. To achieve this sensitivity, two acceptable methods for the detection of human exposure to seven fentanyl analogs and three metabolites were developed using either off-line 96-well plate SPE or on-line SPE. Each system offers different advantages: off-line 96-well plate SPE allows for high throughput analysis of many samples, which is needed for large sample numbers, while on-line SPE removes almost all analyst manipulation of the samples, minimizing the analyst time needed for sample preparation. Both sample preparations were coupled with reversed phase liquid chromatography and isotope dilution tandem mass spectrometry (LC-MS/MS) for analyte detection. For both methods, the resulting precision was within 15%, the accuracy within 25%, and the sensitivity was comparable with the limits of detection ranging from 0.002ng/mL to 0.041ng/mL. Additionally, matrix effects were substantially decreased from previous reports for both extraction protocols. The results of this comparison showed that both methods were acceptable for the detection of exposures to fentanyl analogs and metabolites in urine.
authors.affiliation: Centers for Disease Control and Prevention, 4770 Buford Highway, MS F44, Atlanta, GA 30341, United States.
authors.forename: Rebecca L
authors.initials: RL
authors.lastname: Shaner
authors.affiliation: ORISE Fellow, Centers for Disease Control and Prevention, National Center for Environmental Health, Division of Laboratory Sciences, Atlanta, GA 30341, United States.
authors.forename: Pearl
authors.initials: P
authors.lastname: Kaplan
authors.affiliation: Centers for Disease Control and Prevention, 4770 Buford Highway, MS F44, Atlanta, GA 30341, United States.
authors.forename: Elizabeth I
authors.initials: EI
authors.lastname: Hamelin
authors.affiliation: Centers for Disease Control and Prevention, 4770 Buford Highway, MS F44, Atlanta, GA 30341, United States.
authors.forename: William A
authors.initials: WA
authors.lastname: Bragg
authors.affiliation: Centers for Disease Control and Prevention, 4770 Buford Highway, MS F44, Atlanta, GA 30341, United States. Electronic address: rmj6@cdc.gov.
authors.forename: Rudolph C
authors.initials: RC
authors.lastname: Johnson
mesh_terms: D000701:Analgesics, Opioid / Q000737:chemistry* / Q000378:metabolism / Q000652:urine*; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D005283:Fentanyl / Q000031:analogs & derivatives* / Q000378:metabolism / Q000652:urine*; D006801:Humans; D057230:Limit of Detection; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods
chemical_list: D000701:Analgesics, Opioid; D005283:Fentanyl
keywords: Automation; Fentanyl; Fentanyls; Liquid chromatography; Mass spectrometry; Method development; Solid phase extraction