CAJ | 학술논문

目的建立尿样中挥发性亚硝胺类化合物含量的气相色谱-质谱的检测方法,并应用于实际样本的检测.方法样品采用二氯甲烷进行液液萃取,后取二氯甲烷层进行过滤,于40℃下氮气吹干,使用0.2 ml二氯甲烷定容；利用气相色谱-质谱仪的选择离子监测模式测定9种挥发性亚硝胺,采用外标法定量,并对方法检测限,精密度和准确度进行评价.同时检测了安徽某镇92份居民的尿样中9种挥发性亚硝胺的含量.结果得到9种待测物线性范围较好(2 ～ 200 ng/ml),相关系数为0.9985～ 0.9999,最低检出浓度为0.05～0.50 ng/ml.加标回收率为68％～ 102％,RSD为0.4％～5.5％(n=3),方法检测限为0.001～0.013 ng/ml.92名受检人群N-亚硝基二甲胺(NDMA),N-亚硝基甲基乙基胺(NMEA),亚硝基-二乙基胺(NDEA),N-亚硝基二丙胺(NDPA),N-亚硝基吡咯烷(NPYR),N-亚硝基吗啉(NMOR),N-亚硝基哌啶(NPIP),N-亚硝基二丁胺(NDBA),N-亚硝基二苯胺(NDPhA)检出率依次为71％ (65),74％(68),65％(60),80％(73),92％(85),78％(72),76％(70),87％(80),98％(90)；测得结果分别为(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)、(15.13±3.48) nmol/g肌酐.结论建立了尿样中低含量亚硝胺的气相色谱-质谱检测方法.
목적 건립뇨양중휘발성아초알류화합물함량적기상색보-질보적검측방법,병응용우실제양본적검측.방법 양품채용이록갑완진행액액췌취,후취이록갑완층진행과려,우40℃하담기취간,사용0.2 ml이록갑완정용；이용기상색보-질보의적선택리자감측모식측정9충휘발성아초알,채용외표법정량,병대방법검측한,정밀도화준학도진행평개.동시검측료안휘모진92빈거민적뇨양중9충휘발성아초알적함량.결과 득도9충대측물선성범위교호(2 ～ 200 ng/ml),상관계수위0.9985～ 0.9999,최저검출농도위0.05～0.50 ng/ml.가표회수솔위68％～ 102％,RSD위0.4％～5.5％(n=3),방법검측한위0.001～0.013 ng/ml.92명수검인군N-아초기이갑알(NDMA),N-아초기갑기을기알(NMEA),아초기-이을기알(NDEA),N-아초기이병알(NDPA),N-아초기필각완(NPYR),N-아초기마람(NMOR),N-아초기고정(NPIP),N-아초기이정알(NDBA),N-아초기이분알(NDPhA)검출솔의차위71％ (65),74％(68),65％(60),80％(73),92％(85),78％(72),76％(70),87％(80),98％(90)；측득결과분별위(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)、(15.13±3.48) nmol/g기항.결론 건립료뇨양중저함량아초알적기상색보-질보검측방법.
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.