title: Quantitative analysis of heterocyclic amines in urine by liquid chromatography coupled with tandem mass spectrometry.
abstract: A sensitive, reproducible, and rapid analytical method for the analysis of trace-level heterocyclic amines (HCAs) that are expected to have high levels of human exposure was developed. Liquid-liquid extraction (LLE) with dichloromethane (DCM) followed by solid-phase extraction (SPE) was carried out. Liquid extraction with DCM under basic conditions was efficient in extracting HCAs from urine samples. For further purification, mixed mode cationic exchange (MCX) cartridges were applied to eliminate the remaining interferences after liquid extraction. Separation and quantification were performed by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) in selected reaction monitoring (SRM) mode. The overall recoveries ranged between 71.0% and 113.6% with relative standard deviations (RSDs) of 5.1% to 14.7% for the entire procedure. The limits of detection (LODs) and limits of quantification (LOQs) of the proposed analytical method were in the ranges of 0.04 to 0.10 ng/ml and 0.15 to 0.36 ng/ml, respectively. This method was applied to the analysis of monitoring in urine samples for Korean school children, and the results demonstrated that the method can be used for the trace determination of HCAs in urine samples.
authors.affiliation: Seoul Center, Korea Basic Science Institute, Sungbuk-Ku, Seoul 136-701, Republic of Korea.
authors.forename: Jeoung Hwa
authors.initials: JH
authors.lastname: Shin
authors.affiliation: Seoul Center, Korea Basic Science Institute, Sungbuk-Ku, Seoul 136-701, Republic of Korea.
authors.forename: Yun-Cheol
authors.initials: YC
authors.lastname: Na
authors.affiliation: Seoul Center, Korea Basic Science Institute, Sungbuk-Ku, Seoul 136-701, Republic of Korea.
authors.forename: Joo Hee
authors.initials: JH
authors.lastname: Chung
authors.affiliation: Institute for Drug Research, School of Pharmacy, The Hebrew University, Hadassah Medical School, Jerusalem 91120, Israel.
authors.forename: Shela
authors.initials: S
authors.lastname: Gorinstein
authors.affiliation: Seoul Center, Korea Basic Science Institute, Sungbuk-Ku, Seoul 136-701, Republic of Korea. Electronic address: ygahn@kbsi.re.kr.
authors.forename: Yun Gyong
authors.initials: YG
authors.lastname: Ahn
mesh_terms: D000588:Amines / Q000737:chemistry* / Q000633:toxicity*; D002648:Child; D002853:Chromatography, Liquid; D004781:Environmental Exposure / Q000032:analysis; D006571:Heterocyclic Compounds / Q000737:chemistry*; D006801:Humans; D009153:Mutagens / Q000032:analysis* / Q000737:chemistry*; D018570:Risk Assessment; D053719:Tandem Mass Spectrometry; D016482:Urinalysis / Q000379:methods*
chemical_list: D000588:Amines; D006571:Heterocyclic Compounds; D009153:Mutagens
keywords: Heterocyclic amines; LC–MS/MS; LLE; Solid-phase extraction; Urine