为准确测定卷烟滤嘴截留主流烟气中的主要酚类化合物,通过考察滤嘴切割方式、萃取液、萃取方式、萃取时间等前处理条件,建立了一种快速、准确测定卷烟滤嘴中对苯二酚、间苯二酚、邻苯二酚、苯酚、对甲酚、间甲酚和邻甲酚7种酚类化合物...为准确测定卷烟滤嘴截留主流烟气中的主要酚类化合物,通过考察滤嘴切割方式、萃取液、萃取方式、萃取时间等前处理条件,建立了一种快速、准确测定卷烟滤嘴中对苯二酚、间苯二酚、邻苯二酚、苯酚、对甲酚、间甲酚和邻甲酚7种酚类化合物截留量的高效液相色谱（HPLC）方法,并采用该方法在6家实验室对7种不同滤嘴卷烟样品进行了比对实验。结果表明：1将卷烟抽吸后的滤嘴从烟支端向近嘴端纵向划开后,用50 m L萃取液（1%乙酸＋79%甲醇＋20%水,体积分数）在室温下超声萃取30 min时,可将卷烟滤嘴中截留的7种主要酚类化合物萃取完全。27种酚类化合物在0.04-4.00μg/m L浓度范围内线性关系良好（R2均大于0.999）,回收率为93.35%-104.50%,相对标准偏差（RSD）小于7.3%。36家实验室对7种卷烟样品滤嘴截留的7种酚类化合物检测结果的RSD均小于15%,其中5种酚类化合物在10%以下。该方法适用于卷烟滤嘴截留主流烟气中7种酚类化合物的测定。展开更多
An improved method was developed for the determination of the four major tobacco-specific nitrosamines(TSNAs) in mainstream cigarette smoke. The new method offers decreased sample preparation and analysis time as comp...An improved method was developed for the determination of the four major tobacco-specific nitrosamines(TSNAs) in mainstream cigarette smoke. The new method offers decreased sample preparation and analysis time as compared to traditional methods. This method uses isotope dilution liquid chromatography coupled with a tandem mass spectrometer with electrospray ionization and is significantly more sensitive than traditional methods. It also shows no evidence of artifactual formation of TSNAs. Sample concentrations were determined for four TSNAs in mainstream smoke using two isotopically labeled TSNAs analogues as internal standards. Mainstream smoke was collected on an industry standard 44-mm Cambridge filter pad, extracted with 0.1 mol/L ammonium acetate, purified by solid-phase extraction, and analyzed without further sample cleanup. The analytical column is a 3.9 mm×150 mm Waters Symmertry Shield RP18 column and volume fraction of the mobile phase is 50% methanol, 50% water containing 0.1% acetic acid. The results show that the linear range is 0.5-100.0 mg/L except for N-nitrosoanabasine (NAB) from 0.25 to 50.0 mg/L. The limits of detection are 0.1 mg/L for N-nitrosonornicotine (NNN), 0.08 mg/L for 4-(methylnitrosamino)-1- (3-py-ridyl)-1-butanone (NNK), 0.05 mg/L for N-nitrosoanatabine (NAT) and 0.06 mg/L for NAB. The recoveries of the four TSNAs are from 90.2% to 105.7%.展开更多
文摘为准确测定卷烟滤嘴截留主流烟气中的主要酚类化合物,通过考察滤嘴切割方式、萃取液、萃取方式、萃取时间等前处理条件,建立了一种快速、准确测定卷烟滤嘴中对苯二酚、间苯二酚、邻苯二酚、苯酚、对甲酚、间甲酚和邻甲酚7种酚类化合物截留量的高效液相色谱（HPLC）方法,并采用该方法在6家实验室对7种不同滤嘴卷烟样品进行了比对实验。结果表明：1将卷烟抽吸后的滤嘴从烟支端向近嘴端纵向划开后,用50 m L萃取液（1%乙酸＋79%甲醇＋20%水,体积分数）在室温下超声萃取30 min时,可将卷烟滤嘴中截留的7种主要酚类化合物萃取完全。27种酚类化合物在0.04-4.00μg/m L浓度范围内线性关系良好（R2均大于0.999）,回收率为93.35%-104.50%,相对标准偏差（RSD）小于7.3%。36家实验室对7种卷烟样品滤嘴截留的7种酚类化合物检测结果的RSD均小于15%,其中5种酚类化合物在10%以下。该方法适用于卷烟滤嘴截留主流烟气中7种酚类化合物的测定。
基金Project(2005JC02) supported by China Tobacco Hunan Industrial Corporation Limited
文摘An improved method was developed for the determination of the four major tobacco-specific nitrosamines(TSNAs) in mainstream cigarette smoke. The new method offers decreased sample preparation and analysis time as compared to traditional methods. This method uses isotope dilution liquid chromatography coupled with a tandem mass spectrometer with electrospray ionization and is significantly more sensitive than traditional methods. It also shows no evidence of artifactual formation of TSNAs. Sample concentrations were determined for four TSNAs in mainstream smoke using two isotopically labeled TSNAs analogues as internal standards. Mainstream smoke was collected on an industry standard 44-mm Cambridge filter pad, extracted with 0.1 mol/L ammonium acetate, purified by solid-phase extraction, and analyzed without further sample cleanup. The analytical column is a 3.9 mm×150 mm Waters Symmertry Shield RP18 column and volume fraction of the mobile phase is 50% methanol, 50% water containing 0.1% acetic acid. The results show that the linear range is 0.5-100.0 mg/L except for N-nitrosoanabasine (NAB) from 0.25 to 50.0 mg/L. The limits of detection are 0.1 mg/L for N-nitrosonornicotine (NNN), 0.08 mg/L for 4-(methylnitrosamino)-1- (3-py-ridyl)-1-butanone (NNK), 0.05 mg/L for N-nitrosoanatabine (NAT) and 0.06 mg/L for NAB. The recoveries of the four TSNAs are from 90.2% to 105.7%.
