title: Simultaneous determination of polycyclic musks in blood and urine by solid supported liquid-liquid extraction and gas chromatography-tandem mass spectrometry.
abstract: A rapid, precise and accurate method for the simultaneous determination of 5 polycyclic musks (PCMs) in biological fluids was developed by solid supported liquid-liquid extraction (SLE) coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS). All parameters influencing SLE-GC-MS performance, including electron energy of electron-impact ionization source, collision energy for tandem mass spectrometer when operated in selected-reaction monitoring (SRM) mode, type and volume of elution reagent, nitrogen evaporation time, pH and salinity of sample have been carefully optimized. Eight milliliter of n-hexane was finally chosen as elution reagent. Blood and urine sample could be loaded into SLE cartridge without adjusting pH and salinity. Deuterated tonalide (AHTN-d3) was chosen as internal standard. The correlation coefficient (r(2)) of the calibration curves of target compounds ranged from 0.9996 to 0.9998. The dynamic range spanned over two orders of magnitude. The limit of detection (LOD) of target compounds in blood and urine ranged from 0.008 to 0.105μgL(-1) and 0.005 to 0.075μgL(-1), respectively. The developed procedure was successfully applied to the analysis of PCMs in human blood and urine obtaining satisfying recoveries on low, medium and high levels. The method was compared with SLE-GC-MS and shown one to two orders of magnitude improvement in sensitivity.
authors.affiliation: MOE Key Laboratory of Aquatic Product Safety, Instrumental Analysis & Research Center, Sun Yat-Sen University, Guangzhou 510275, PR China. Electronic address: liuht@mail.sysu.edu.cn.
authors.forename: Hongtao
authors.initials: H
authors.lastname: Liu
authors.affiliation: Department of Obstetrics and Gynecology, Nan Fang Hospital, Southern Medical University, Guangzhou 510515, PR China. Electronic address: lphuang2006@126.com.
authors.forename: Liping
authors.initials: L
authors.lastname: Huang
authors.affiliation: MOE Key Laboratory of Aquatic Product Safety, Instrumental Analysis & Research Center, Sun Yat-Sen University, Guangzhou 510275, PR China.
authors.forename: Yuxin
authors.initials: Y
authors.lastname: Chen
authors.affiliation: MOE Key Laboratory of Aquatic Product Safety, Instrumental Analysis & Research Center, Sun Yat-Sen University, Guangzhou 510275, PR China.
authors.forename: Liman
authors.initials: L
authors.lastname: Guo
authors.affiliation: MOE Key Laboratory of Aquatic Product Safety, Instrumental Analysis & Research Center, Sun Yat-Sen University, Guangzhou 510275, PR China.
authors.forename: Limin
authors.initials: L
authors.lastname: Li
authors.affiliation: MOE Key Laboratory of Aquatic Product Safety, Instrumental Analysis & Research Center, Sun Yat-Sen University, Guangzhou 510275, PR China.
authors.forename: Haiyun
authors.initials: H
authors.lastname: Zhou
authors.affiliation: MOE Key Laboratory of Aquatic Product Safety, Instrumental Analysis & Research Center, Sun Yat-Sen University, Guangzhou 510275, PR China; School of Life Sciences, Sun Yat-Sen, University, Guangzhou 510275, PR China. Electronic address: cesltg@mail.sysu.edu.cn.
authors.forename: Tiangang
authors.initials: T
authors.lastname: Luan
mesh_terms: D000328:Adult; D001578:Benzopyrans / Q000097:blood / Q000737:chemistry / Q000652:urine; D005260:Female; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D006863:Hydrogen-Ion Concentration; D057230:Limit of Detection; D016014:Linear Models; D059625:Liquid-Liquid Extraction / Q000379:methods*; D010476:Perfume / Q000032:analysis / Q000737:chemistry; D011084:Polycyclic Aromatic Hydrocarbons / Q000097:blood / Q000737:chemistry / Q000652:urine; D015203:Reproducibility of Results; D012965:Sodium Chloride; D053719:Tandem Mass Spectrometry; D055815:Young Adult
chemical_list: D001578:Benzopyrans; D010476:Perfume; D011084:Polycyclic Aromatic Hydrocarbons; C033119:galaxolide; D012965:Sodium Chloride
keywords: Gas chromatography–tandem mass spectrometry (GC–MS/MS); Pharmaceuticals and personal care products (PPCPs); Polycyclic musks (PCMs); Solid supported liquid–liquid extraction (SLE)