title: [Determination of volatile nitrosamines in urine through gas chromatography-mass spectrometry].
abstract: OBJECTIVE
  To establish a detection method based on gas chromatography-mass spectrometry (GC-MS) for concentrations of volatile nitrosamine compounds in urine, and apply it to the test of real samples.
  
  
  METHODS
  Target compounds dichloromethane in urine samples was extracted with dichloromethane through liquid-liquid extraction, then the dichloromethane extract was filtrated, evaporated with nitrogen at 40°C to dryness, and the volume was set with 0.2 ml dichloromethane. Analysis of nine volatile nitroso-compounds were performed with GC-MS under selected ion monitoring mode, external reference method was used for quantification, and the detection limit, repeatability and sensitivity were evaluated. In addition, nine volatile nitroso-compounds of 92 urine samples in a town of Anhui province were measured.
  
  
  RESULTS
  A good linear range of 2 - 200 ng/ml (with correlation coefficient 0.9985 - 0.9999) were obtained for the above mentioned nine kinds of analyte, and the lowest examination concentration was 0.05 - 0.50 ng/ml. The addition standard recoveries were 68%-102% with the RSD of 0.4% - 5.5% (n = 3). The detection limits were 0.001 - 0.013 ng/ml urine. The detection rate of N-nitrosodimethylamine (NDMA), N-nitrosomethylethylamine (NMEA), N-nitrosodiethylamine (NDEA), N-nitrosodi-n-propylamine (NDPA), N-nitrosopyrrolidine (NPYR), N-nitrosomorpholine (NMOR), N-nitrosopiperidine (NPIP), N-nitrosodi-n-butylamine (NDBA) and N-nitrosodiphenylamine (NDPhA) were 71% (65), 74% (68), 65% (60), 80% (73), 92% (85), 78% (72), 76% (70), 87% (80), 98% (90), respectively, with the results (0.27 ± 0.12), (0.75 ± 0.29), (0.06 ± 0.02), (0.16 ± 0.07), (23.66 ± 5.18), (1.01 ± 0.35), (0.38 ± 0.11), (2.47 ± 0.52) and (15.13 ± 3.48) nmol/g creatinine.
  
  
  CONCLUSIONS
  A gas chromatography-mass spectrometry detect method was developed for low level volatile nitrosamines in urine samples.
authors.affiliation: Department of Hygienic Analysis and Detection, Center for Disease Control and Prevention of Changjiang River Administration and Navigational Affairs, Ministry of Transport, Wuhan 430019, China.
authors.forename: Run-zheng
authors.initials: RZ
authors.lastname: Guo
authors.forename: Yan-jian
authors.initials: YJ
authors.lastname: Wan
authors.forename: Chun-jiang
authors.initials: CJ
authors.lastname: Wu
authors.forename: Yan
authors.initials: Y
authors.lastname: Zhang
authors.forename: Qi-hui
authors.initials: QH
authors.lastname: Huang
authors.forename: Hai-xia
authors.initials: HX
authors.lastname: Li
authors.forename: Xu
authors.initials: X
authors.lastname: Wang
authors.forename: Zhong-hou
authors.initials: ZH
authors.lastname: Cao
authors.forename: Yu-hua
authors.initials: YH
authors.lastname: Mao
authors.forename: Jie
authors.initials: J
authors.lastname: Shen
authors.forename: Wei
authors.initials: W
authors.lastname: Xia
authors.forename: Yuan-yuan
authors.initials: YY
authors.lastname: Li
authors.forename: Shun-qing
authors.initials: SQ
authors.lastname: Xu
mesh_terms: D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D009602:Nitrosamines / Q000652:urine*; D016482:Urinalysis / Q000379:methods*; D055549:Volatile Organic Compounds / Q000652:urine
chemical_list: D009602:Nitrosamines; D055549:Volatile Organic Compounds