卷烟主流烟气总粒相物中挥发性和半挥发性有机酸的分析

采用二氯甲烷萃取、N,O-双(三甲基硅基)三氟乙酰胺硅烷化、反-2-己烯酸和肉桂酸作内标,接预分离柱和选择离子检测GC/MS法同时测定了卷烟主流烟气中的甲酸、乙酸和二十酸等30种有机酸。方法的回收率为74.3%～101.8%,RSD均小于10%。并采用该法测定了10个牌号国产烤烟型卷烟烟气中有机酸含量。该法适于批量卷烟主流烟气总粒相物中挥发性和半挥发性有机酸的快速分析。     

HPLC-MS/MS检测卷烟主、侧流烟气中的杂环胺

建立了MCX阳离子柱固相萃取净化、大气压电离模式下液相色谱串联四极杆质谱测定8种杂环胺类的方法,并采用该方法测定了8种卷烟样品主、侧流烟气中这8种杂环胺的含量。结果表明:①方法的检测限为0.042～2.8ng/支,回收率为68%～108%,RSD为1.6%～8.8%;②这些卷烟样品主、侧流烟气中均检测到MeAαC,AαC,Trp-p-1,Trp-p-2;③卷烟主、侧流烟气中的AαC,MeAαC,Trp-p-2和Trp-p-1释放量之间均相关;AαC与MeAαC,Trp-p-2与Trp-p-1的相关性显著;④除1种卷烟样品外,其余卷烟样品侧流烟气中杂环胺的释放量都高于主流烟气。     

卷烟烟气中稠环芳烃的分析研究

本项研究建立了一种测定卷烟烟气中稠环芳烃的分析方法--气质联用法.优化了方法的前处理过程、仪器分析条件,对分析方法的重复性、回收率、检测限进行了研究.确定了环己烷萃取卷烟烟气总粒相物中的稠环芳烃,萃取液经硅胶固相萃取柱净化,用气相色谱-质谱联用仪定量检测苯并[a]芘、苯并[a]蒽和Chrysene 3种稠环芳烃含量的分析方法.该检测方法设计合理,稳定性和重复性好、准确性和精确性高,具有较好的可操作性和推广性.本项目应用该方法对国内外较有代表性的81种卷烟样品中苯并[a]芘、苯并[a]蒽和Chrysene进行了系统的分析测定,研究了国内外混合型与烤烟型卷烟中苯并[a]芘等稠环芳烃含量分布的规律,讨论了卷烟烟气中苯并[a]芘、苯并[a]蒽和Chrysene之间的含量关系及其与总粒相物、焦油的关系.     

超声萃取-快速HPLC法测定卷烟主流烟气中的苯酚、甲酚和苯二酚

建立了超声萃取-快速高效液相色谱同时测定卷烟主流烟气中的苯酚、甲酚和苯二酚的方法。即用1%的醋酸水溶液于室温下对捕集了烟气粒相物的剑桥滤片超声萃取20min,将萃取液用0.45μm滤膜过滤后,滤液直接用配置荧光检测器的快速分离柱-高效液相色谱进行分析。并应用该法测定了10种国产烤烟型和10种混合型卷烟主流烟气中的挥发酚,结果表明:①该法的相对标准偏差为1.92%～4.62%,回收率97.9%～100.3%,检测限5.74～14.70ng/支,分析时间6min;②烤烟型卷烟主流烟气中苯二酚、苯酚的含量明显高于混合型卷烟,而甲酚的含量整体上略高于混合型;③同类型卷烟主流烟气中挥发酚含量高低的次序为p-苯二酚>o-苯二酚>苯酚>(m、o)-甲酚>p-甲酚>m-苯二酚。该法适合批量卷烟主流烟气中苯酚、甲酚和苯二酚的快速分析。     

卷烟主流烟气中羰基化合物的改进分析方法

选择2，4-二硝基苯肼作为羰基化合物的衍生化试剂，采用高效液相色谱（HPLC）分析卷烟烟气中主要8种羰基化合物。卷烟主流烟气通过经2，4-二硝基苯肼（DNPH）酸性溶液处理的剑桥滤片进行捕集，烟气中的羰基化合物与DNPH反应生成相应的2，4-二硝基苯腙衍生物，经乙腈萃取后，采用配备紫外检测器的高效液相色谱进行定量分析。与以往的分析方法相比，该方法防止了丙烯醛衍生化合物的进一步反应，提高了分析的准确性。评价了该方法测定烟气中8种羰基化合物的重复性、回收率及检测限，采用该方法测定了肯塔基参考卷烟2R4F和部分国内外卷烟。     

卷烟主流烟气中烟草特有亚硝胺的液质联用分析

采用0.1mol/L醋酸铵水溶液萃取、固相萃取纯化和高效液相色谱-三级四极杆质谱法测定了12种卷烟样品主流烟气中4种烟草特有亚硝胺(TSNAs)。结果表明:①NNN、NAT、NNK和NAB的检测限分别为0.07、0.05、0.05和0.04ng/mL,回收率在94.0%～103.5%之间,相对标准偏差分别为3.02%、4.19%、6.10%和6.62%;②2种进口混合型卷烟主流烟气中的总TSNAs均远远高于10种国产烤烟型卷烟。该法适合批量卷烟主流烟气中TSNAs的定量分析。     

卷烟烟气粒相物中挥发性香味成分的分析研究

为建立一种卷烟烟气粒相物中挥发性香味成分的分析方法,以挥发性香味成分的测定值为指标,考察了不同萃取剂对测定结果的影响,最终确定以甲醇为萃取剂;通过对样品进行GC/MS分析,进行质谱检索,结合匹配度,确定了样品中的目标组分;将同种卷烟样品平行测定5次,卷烟烟气粒相挥发香味成分的相对标准偏差在1.98%~7.88%,所测烟气粒相物挥发性香味成分的平均回收率在85.26%~105.59%之间,说明该优化方法可行,适于卷烟烟气粒相物中挥发性香味成分的分析。     

中心切割二维气相色谱法测定卷烟主流烟气中的硝基苯

建立了环己烷萃取、硅胶固相萃取柱净化和中心切割二维气相色谱法测定卷烟主流烟气粒相物中硝基苯的方法,并采用该法测定了6种卷烟样品主流烟气中的硝基苯释放量。结果表明:①中心切割技术有效提高了色谱的分离能力,使得痕量硝基苯可以从复杂的烟气基质中分离出来,分离效果明显优于一维色谱;②方法的检测限为1.28 ng/mL,相对标准偏差(RSD)6.82%,回收率87.6%;③6种卷烟主流烟气中硝基苯的释放量为0.091~1.66 ng支/。     

原位萃取法测定加热卷烟气溶胶中的水分和焦油

为准确测定加热卷烟气溶胶中的水分和焦油,设计并开发了吸烟机捕集器原位萃取仪,通过在加热卷烟抽吸后,直接进行金属捕集器内部原位萃取,建立原位萃取-气相色谱测定加热卷烟气溶胶中水分的分析方法。结果表明:①方法的回收率在95.4%~104.6%之间,RSD在3.72%~6.09%之间,检出限为0.16 mg/支。②与传统的振荡萃取法相比,在ISO抽吸模式下原位萃取法的水分测定值增加15.95%~22.16%,HCI抽吸模式下增加38.34%~40.37%。③原位萃取不影响烟碱、1, 2-丙二醇和丙三醇等加热卷烟气溶胶主要成分的测定;原位萃取同样也适用于传统卷烟烟气焦油释放量的测定。该方法适用于加热卷烟气溶胶中水分、焦油、烟碱、1, 2-丙二醇和丙三醇的准确测定。      

高效液相色谱法测定卷烟滤嘴中截留的主要酚类化合物

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。     

烟用香精中薄荷醇的气相色谱/质谱分析

采用保留时间比对法和选择离子(81amu)气相色谱/质谱法定性定量分析了烟用香精中的薄荷醇.方法的检测限为0.0028mg/mL,平均回收率为98.52%,RSD为2.41%.     

Rapid determination of benzo(a)pyrene in processed meat and fish samples by second-derivative constant-energy synchronous fluorescence spectrometry

A simple, rapid and cost-effective method has been established for the determination of the quantity of benzo(a)pyrene (BaP), one of the most carcinogenic polycyclic aromatic hydrocarbons (PAHs), in roasted, smoked and charcoal grilled foods. Second-derivative constant-energy synchronous fluorescence spectrometry (DCESFS) improves the spectral resolution and selectivity of the fluorescence method. By using this method, processed meat, fish and some other food samples were analysed without resorting to complex pre-separation and purification procedures. The method was found to have a recovery of 97.7% ± 4.3%. The limit of detection (LOD) for BaP was 0.14 μg kg?1, far below the regulatory limit (1.0 μg kg?1) for BaP in food samples specified by the European Union. A certified reference material (Coconut oil, BCR?-458) was used to confirm the validity of the proposed method. The results suggest that the measurements are in a good agreement with the certified BaP concentrations (5.4% deviation). The results obtained by the proposed method for analysing BaP in food samples correlated well with those obtained by GC/MS.     

卷烟主流烟气中苯并[a]芘的HPLC测定

先用乙醇 +乙醚混合溶剂萃取卷烟烟气总粒相物 (TPM) ,再用中性氧化铝柱层析 ,然后 ,利用配有ODS -C18色谱柱的高效液相色谱仪 ,在以 90 %甲醇 + 10 %水为流动相 ,流速为 1mL min ,激发波长 2 86nm和发射波长 4 30nm的条件下测定了TPM中的苯并 [a]芘含量。苯并 [a]芘的回收率≥ 91.2 % ,方法的RSD <5 %。并采用该方法测定了 10种不同焦油量卷烟主流烟气中的苯并 [a]芘含量。结果表明 ,就所测定的卷烟而言 ,①在焦油量相近的情况下 ,混合型卷烟烟气中的苯并 [a]芘含量较烤烟型卷烟的低 8.2 9%～ 19.5 9% ;②无论是烤烟型还是混合型卷烟 ,随着卷烟焦油量的降低 ,虽然焦油中的苯并[a]芘总量明显降低 ,但单位量焦油中的苯并 [a]芘含量却明显增大。     

Rapid determination of benzo(a)pyrene in processed meat and fish samples by second-derivative constant-energy synchronous fluorescence spectrometry

A simple, rapid and cost-effective method has been established for the determination of the quantity of benzo(a)pyrene (BaP), one of the most carcinogenic polycyclic aromatic hydrocarbons (PAHs), in roasted, smoked and charcoal grilled foods. Second-derivative constant-energy synchronous fluorescence spectrometry (DCESFS) improves the spectral resolution and selectivity of the fluorescence method. By using this method, processed meat, fish and some other food samples were analysed without resorting to complex pre-separation and purification procedures. The method was found to have a recovery of 97.7%?±?4.3%. The limit of detection (LOD) for BaP was 0.14?µg?kg^–1, far below the regulatory limit (1.0?µg?kg^–1) for BaP in food samples specified by the European Union. A certified reference material (Coconut oil, BCR®-458) was used to confirm the validity of the proposed method. The results suggest that the measurements are in a good agreement with the certified BaP concentrations (5.4% deviation). The results obtained by the proposed method for analysing BaP in food samples correlated well with those obtained by GC/MS.     

Determination of low-level pesticide residues in agricultural products by ion-trap GC/MS/MS

The objective of this study was to elucidate the utility of ion-trap GC/MS/MS for the analysis of pesticides in extracted matrices from various agricultural products. Identification and quantitative analysis of pesticides in matrices were performed by quadrupole GC/MS and ion-trap GC/MS/MS. Chlorpyrifos was added to the matrix of spinach, soybean in the pod or corn, and aldrin, dieldrin, endrin, alpha-BHC, beta-BHC, gamma-BHC, delta-BHC, p,p'-DDD, p,p'-DDE, o,p'-DDT and p,p'-DDT were added to each matrix of green tea, black tea or oolong tea. Although most of the pesticides in the matrix could not be determined by quadrupole GC/MS-Scan analysis at 0.1 microgram/mL, every pesticide was identified from the mass spectrum using ion-trap GC/MS/MS at the same concentration. The quantitation limit of every pesticide in each matrix by ion-trap GC/MS/MS analysis was higher than that by GC/MS-SIM analysis. The calibration curves obtained by GC/MS/MS were linear in the range of 0.01-0.25 microgram/mL of each pesticide. The recoveries of each pesticide from four kinds of samples spiked at the levels of 0.01 ppm to 0.02 ppm in extracts were 61.2-138.3% with SD values in the range from 1.2 to 15.4%. This study revealed that ion-trap GC/MS/MS was useful for the identification and quantitative analysis of low-level pesticides residues in matrices of agricultural products.     

基于静态顶空-GC/MS的加热卷烟用滤嘴载香颗粒评价研究

[目的]建立一种基于静态顶空-GC/MS的加热卷烟用滤嘴载香颗粒评价方法.[方法]采用静态顶空-GC/MS考察不同温度下4种载香颗粒中12种香味成分的释放行为,通过CH2Cl2萃取和GC/MS分析添加4种载香颗粒的加热卷烟主流烟气中香味成分释放量验证静态顶空-GC/MS评价结果.[结果]载香颗粒在加热卷烟实际抽吸降温段...     

几种国内外混合型卷烟烟丝中香味物质的分析比较

本采用同时蒸馏萃取（SDE）的前处理分离方法，以及气相色谱和气质谱联用分析鉴定技术，对9种国内外混合型卷烟烟丝中的半挥发性酸性，碱性和中性成分进行了分析研究，共鉴定出37种碱性成分，83种中性成分和12种酸性成分。采用内标法定量测定了烟丝中的噻唑、吡啶、四甲基吡嗪，吡咯和吲哚等18种碱性香味成分，芳樟醇，二氢大马酮，香味基丙酮，氧化异佛尔酮和二氢猕猴桃内酯等47种中性香味成分；乙醇、3－甲基戊酸、十四酸和棕榈酸等12种酸性成分。以及酸性，碱性和中性成分的总量，评价了该方法的重复性和前处理过程的回收率，研究结果表明，烟丝中中性成分总量的平均值国外卷烟比国产卷烟略高，烟丝中酸性成分总量的平均值国外卷烟化国产卷烟略低，烟丝中碱性成分总量的平均值（烟碱除外）国外卷烟是国产卷烟的2．2倍。     

烟草二氧化碳超临界萃取物的初步研究

初步探索了二氧化碳超临界流体萃取烟草成分的技术参数,采用气相色谱仪和气质联用仪分析了烟草萃取物.结果表明,二氧化碳超临界萃取物以非极性和弱极性化合物为主.另外对上海烟草(集团)公司的4种牌号卷烟产品萃取物的相对定量分析结果表明,"中华"牌卷烟的萃取物含量最高,"双喜"次之,"牡丹"第三,"前门"的最低.