摘要
建立了水蒸气蒸馏提取，活性炭柱固相萃取，气相色谱-串联质谱（GC-MS／MS）检测火腿中8种N-亚硝胺的新方法。样品经水蒸气蒸馏提取，馏出液经Sep-PakAC-2活性炭柱固相萃取进行净化与富集，二氯甲烷洗脱，以多重反应监测（MRM）方式进行GC-MS／MS检测。在考察的浓度范围内（1～400ng／mL）方法线性良好，R^2〉0．9995，除N-二甲基亚硝胺（NDMA）和N．亚硝基甲乙胺（NMEA）检出限≤0．1ng／g外，其它分析物的检出限为≤0．04ng／g；在0．3，3和10μ/kg3个水平的添加回收率为78．7％～118．2％，除N-亚硝基吗啉（NMOR）回收率略低，为45．2％-58．2％，相对标准偏差为2．5％～21％。应用该方法对市售的4种火腿进行检测，结果表明NDMA和N-亚硝基吡咯烷（NPYR）是主要的挥发性N-亚硝胺，含量分别为〈0．30ng／g和0．56-0．99ng／g，N-二乙基亚硝胺（NDEA）、NMOR和N一二丁基亚硝胺（NDBA）均有检出，但含量低于定量限，NMEA、N-二丙基亚硝胺（NDPA）和N-亚硝基哌啶（NPIP）未检出。
A new method has been developed for the determination of eight volatile N-nitrosamines in ham products based on steam distillation combined with active carbon solid phase extraction by gas chromatography-tandem mass spectrometry. In this method, volatile N-nitrosamines were extracted by steam distillation and the distillate was cleaned and concentrated in a Sep-Pak AC-2 cartridge and eluted with dichloromethane （DCM）. Mass spectrometry was performed with multiple reaction monitoring （MRM）. Validation data revealed that the calibration curve of eight N-nitrosamines were linear in the range of 1 -400 ng/mL with a good correlation coefficient （R2 ） of 〉 0.9995, the limits of detection （LODs） were no more than 0. 1 ng/g for N-nitrosodimethylamine（NDMA） and N-nitrosomethylethylamine （NMEA）, no more than 0.04 ng/g for other analytes. The recoveries at the spiked levels of 0. 3,3 and 10 txg/kg were 78.7% -118.2% with the relative standard deviations of 2. 5% -21%, except the recovery of N-nitrosomorpholine （NMOR） was lower （45.2% - 58.2% ）. The method was applied to detect four types of commercial ham products. The results showed that NDMA and N-nitrosopyrrolidine （NPYR） were the major volatile N-nitrosamines, concentrations were less than 0.3 ng/g and 0.56 - 0.99 ng/g, respectively; N-nitrosodiethylamine （ NDEA ）, NMOR and N-nitrosodibutylamine （NDMA） were detected, but the contents were less than the quantitative limit. NMEA, N-nitrosadipropylamine （NDPA） and N-nitrosopiperidine （NPIP） were not detected.
出处
《分析试验室》
CAS
CSCD
北大核心
2015年第12期1475-1479,共5页
Chinese Journal of Analysis Laboratory
基金
北京市教委项目(KM201310020009,PXM2014-014207-000001)资助
关键词
气相色谱-串联质谱
N-亚硝胺
火腿
水蒸气蒸馏
活性碳柱固相萃取
Gas chromatography-tandem mass spectrometry （GC-MS/MS）
N-nitrosamines
Ham products
Steam distillation
Active carbon solid phase extraction
