[Determination of volatile nitrosamines in urine through gas chromatography-mass spectrometry].

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 ℃ 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. Key words: Nitrosamines;  Urine;  Gas chromatography-mass spectrometry