title: Analysis of twenty phenolic compounds in human urine: hydrochloric acid hydrolysis, solid-phase extraction based on K2CO 3-treated silica, and gas chromatography tandem mass spectrometry.
abstract: This study developed a new method for the analysis of 20 phenolic compounds in human urine. The urine samples were prepared by hydrochloric acid (HCl) hydrolysis, liquid-liquid extraction (LLE), and solid-phase extraction (SPE) cleanup. We found that HCl hydrolysis is of similar effectiveness to, and much cheaper than, the traditional enzymatic method. Vanillic acid was co-eluted with butyl paraben and interfered with the determination of butyl paraben in urine. K2CO3-treated-silica-gel SPE was designed to efficiently eliminate interference from the endogenous organic acids (especially vanillic acid) in urine. After derivatization, the samples were analyzed by large-volume-injection gas chromatography-tandem mass spectrometry (LVI-GC-MS-MS). Good linearity (R (2) ≥ 0.996) was established in the range 0.1-100 ng mL(-1) for all analytes. Method detection limits (MDLs) were 0.7-9.8 pg mL(-1). Intraday (n = 5) and interday (n = 5 days) validation was performed, with satisfactory accuracy (recovery: 70-126 % and 73-107 %, respectively) and precision (RSD ≤ 19 %) at two levels (low: 0.1 and 0.5 ng mL(-1); high: 5 and 10 ng mL(-1)). The method was used in a population study and achieved more than 85 % detection for most analytes; mean analyte concentrations were in the range 0.01-185 ng mL(-1). The method is suitable for the analysis of multiple phenolic metabolites in human urine.
authors.affiliation: School of Public Health/ MOE Key Lab for Public Health, Fudan University, Shanghai, 200032, China.
authors.forename: Dasheng
authors.initials: D
authors.lastname: Lu
authors.forename: Chao
authors.initials: C
authors.lastname: Feng
authors.forename: Dongli
authors.initials: D
authors.lastname: Wang
authors.forename: Yuanjie
authors.initials: Y
authors.lastname: Lin
authors.forename: Ho Sai Simon
authors.initials: HS
authors.lastname: Ip
authors.forename: Jianwen
authors.initials: J
authors.lastname: She
authors.forename: Qian
authors.initials: Q
authors.lastname: Xu
authors.forename: Chunhua
authors.initials: C
authors.lastname: Wu
authors.forename: Guoquan
authors.initials: G
authors.lastname: Wang
authors.forename: Zhijun
authors.initials: Z
authors.lastname: Zhou
mesh_terms: D000328:Adult; D002254:Carbonates / Q000737:chemistry*; D002675:Child, Preschool; D002849:Chromatography, Gas / Q000379:methods*; D006801:Humans; D006851:Hydrochloric Acid / Q000737:chemistry*; D006868:Hydrolysis; D007223:Infant; D010636:Phenols / Q000652:urine*; D011188:Potassium / Q000737:chemistry*; D015203:Reproducibility of Results; D012822:Silicon Dioxide / Q000737:chemistry*; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods
chemical_list: D002254:Carbonates; D010636:Phenols; D012822:Silicon Dioxide; C037593:potassium carbonate; D006851:Hydrochloric Acid; D011188:Potassium