Guo Run-zheng, Wan Yan-jian, Wu Chun-jiang, Zhang Yan, Huang Qi-hui, Li Hai-xia, Wang Xu, Cao Zhong-hou, Mao Yu-hua, Shen Jie, Xia Wei, Li Yuan-yuan, Xu Shun-qing
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.
Zhonghua Yu Fang Yi Xue Za Zhi. 2013 Mar;47(3):270-3.
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.
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.
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.
A gas chromatography-mass spectrometry detect method was developed for low level volatile nitrosamines in urine samples.
建立一种基于气相色谱 - 质谱联用（GC - MS）的尿液中挥发性亚硝胺化合物浓度检测方法，并将其应用于实际样品检测。
采用液 - 液萃取法，用二氯甲烷提取尿液样品中的目标化合物二氯甲烷，然后对二氯甲烷提取物进行过滤，在40℃下用氮气吹干，用0.2 ml二氯甲烷定容。在选择离子监测模式下用GC - MS对9种挥发性亚硝基化合物进行分析，采用外标法进行定量，并评估检测限、重复性和灵敏度。此外，对安徽省某镇92份尿液样品中的9种挥发性亚硝基化合物进行了测定。
上述9种分析物的线性范围良好，为2 - 200 ng/ml（相关系数为0.9985 - 0.9999），最低检测浓度为0.05 - 0.50 ng/ml。加标回收率为68% - 102%，相对标准偏差为0.4% - 5.5%（n = 3）。尿液的检测限为0.001 - 0.013 ng/ml。N - 亚硝基二甲胺（NDMA）、N - 亚硝基甲乙胺（NMEA）、N - 亚硝基二乙胺（NDEA）、N - 亚硝基二正丙胺（NDPA）、N - 亚硝基吡咯烷（NPYR）、N - 亚硝基吗啉（NMOR）、N - 亚硝基哌啶（NPIP）、N -亚硝基二正丁胺（NDBA）和N - 亚硝基二苯胺（NDPhA）的检出率分别为71%（65份）、74%（68份）、65%（60份）、80%（73份）、92%（85份）、78%（72份）、76%（70份）、87%（80份）、98%（90份），结果分别为（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）和（15.13±3.48）nmol/g肌酐。
建立了一种气相色谱 - 质谱联用检测尿液中低水平挥发性亚硝胺的方法。
