PDF(Pubmed)
Abstract：
Tobacco specific nitrosamines (TSNAs) are highly carcinogenic by-products in tobacco samples, and their presence is regulated by the Food and Drug Administration. Molecularly imprinted polymers (MIPs) are synthetic polymers that have been \"imprinted\" with a template analyte in a co-polymer system, and can selectively extract analytes from complex matrices. MIPs can be incorporated into online systems, replacing traditional high performance liquid chromatography (HPLC) columns. MIP material specific for TSNAs was packed into an empty HPLC column using a slurry packing technique. The developed method with the MIP-packed HPLC column was validated on a LC-MS/MS system for the quantitation of N-nitrosonornicotine (NNN) and 4- (methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK) in commercial tobacco products. The method was linear over .1-10 ng/ml (.4-10 μg/g) for NNN and NNK. The limit of detection (LOD) was .03 ng/ml (12 μg/g) and the limit of quantitation (LOQ), .1 ng/ml (.4 μg/g). All column uniformity parameters with the exception of theoretical plate number were within the accepted criteria (% RSD values <15%). Theoretical plate number was <250, owing to the large (50 μm) sized MIP particles. Twenty-six tobacco products contained TSNA concentrations that were consistent with reported literature values. The TSNA-MIP based HPLC column effectively replaced a traditional reverse phase HPLC column, and was used for the direct analysis of nicotine and tobacco products without extensive sample preparation prior to instrumental analysis.
摘要：
烟草特有的亚硝胺(TSNA)是烟草样品中高度致癌的副产品,他们的存在受到食品和药物管理局的监管。分子印迹聚合物（MIP）是在共聚物系统中用模板分析物“印迹”的合成聚合物，并且可以从复杂的基质中选择性地提取分析物。MIP可以并入在线系统，取代传统的高效液相色谱(HPLC)柱。使用浆液填充技术将对TSNA特异的MIP材料填充到空的HPLC柱中。在LC-MS/MS系统上验证了使用MIP填充的HPLC色谱柱开发的方法，用于定量市售烟草产品中的N-亚硝胺尼古丁（NNN）和4-（甲基亚硝胺）-1-（3-吡啶基）-1-丁酮（NNK）。对于NNN和NNK，该方法在0.1-10ng/ml（.4-10μg/g）范围内呈线性关系。检测限（LOD）为0.03ng/ml（12μg/g），定量限（LOQ），.1ng/ml（.4μg/g）。除理论塔板数外,所有柱均匀性参数均在可接受的标准范围内(%RSD值<15%)。由于大(50μm)尺寸的MIP颗粒,理论塔板数<250。26种烟草产品含有与文献报道值一致的TSNA浓度。基于TSNA-MIP的HPLC柱有效地取代了传统的反相HPLC柱，并用于直接分析尼古丁和烟草产品，而无需在仪器分析之前进行大量样品制备。
