【摘要】 建立氢氧化钡处理,活性炭柱固相萃取,气相色谱-串联质谱法(GC-MS/MS)检测腌制蔬菜中挥发性N-亚硝胺的新方法。将10 g腌制蔬菜样品加入N-二甲基亚硝胺-d6和N-二丙基亚硝胺-d14内标于50 mL离心管中,经80℃密闭处理1h,离心分离,活性炭柱固相萃取,以DB-1701柱(30 m×0.25 mm×0.25μm)气相色谱分离,串联质谱多重反应监测模式进行检测。结果表明,本法可实现对批量腌制蔬菜样本中7种N-亚硝胺的检测,其中N-二丙基亚硝胺(NDPA)的检出限和定量限分别≤0.08 ng/g和≤0.2 ng/g,N-二甲基亚硝胺(NDMA)等其它6种N-亚硝胺检出限和定量限分别≤0.04 ng/g和≤0.1 ng/g;考察质量浓度范围内(1～100 ng/mL),线性良好,R2≥0.9993;0.1,1.0和5.0 ng/g三水平的加标回收率为82.1%～125.6%,相对标准偏差为0.10%～11.8%。对超市腌制蔬菜的抽样(n=46)监测表明,NDMA、N-亚硝基吗啉(NMOR)和N-亚硝基吡咯烷(NPYR)检出率为100%,N-二乙基亚硝胺(NDEA)、NDPA、N-亚硝基哌啶(NPIP)的检出率为71%～88%,N-甲乙基亚硝胺(NMEA)未检出;除NPYR含量较高,最高值为4.71 ng/g外,其它N-亚硝胺含量均在1 ng/g以下;腌制蔬菜中N-亚硝胺处于较安全水平。更多还原

【Abstract】 A new method was developed for determination of seven N-nitrosamines in pickled vegetables by gas chromatography-mass spectrometry with barium hydroxide treatment and active carbon solid phase extraction. With N-nitrosodimethylamine-d6 and N-nitrosadipropylamine-d14 as internal standards, a 10 g pickled vegetables sample was treated by barium hydroxide solution at 80 ℃ in a 50 mL tighten capped plastic centrifugation tube for 1 h. Next, the sample solution was centrifuged and the supernatant was cleaned up and concentrated with active carbon cartridge. The chromatographic separation was carried on a DB-1701 column(30 m×0.25 mm×0.25 μm) and detection was performed with tandem mass spectrometry at multiple reactions monitoring mode. Limit of detection and quantification of N-nitrosadipropylamine(NDPA) was less than 0.08 and 0.2 ng/g respectively, and that of NDMA and others N-nitrosamines were less than 0.04 and 0.1 ng/g respectively. The calibration curves showed good linearity in the investigating range of1-100 ng/mL with the correlation coefficients not less than 0.9993. The recoveries at the spiked levels of 0.1,1 and 5 ng/g were 82.1%-125.6% with the relative standard deviations of 0.10%-11.9%. Pickled vegetables samples(n=46) from a supermarket were monitored. It was found that NDMA, N-nitrosomorpholine(NMOR) and N-nitrosopyrrolidine(NPYR)were detected with the ratio of 100%, N-nitrosodiethylamine(NDEA), NDPA and N-nitrosopiperidine(NPIP) were detected with the ratio of 71%-88%, N-nitrosomethylethylamine(NMEA) was not detected. Among of these analytes,NPYR has a relative higher content than others, the highest content determined was 4.71 ng/g; the contents of other Nnitrosamines were blow 1 ng/g. The levels of N-nitrosamines monitored in the investigating pickled vegetables were safety.更多还原