主流烟气中芳香胺的提取、衍生条件的优化及市售卷烟芳香胺含量的GC/MS测定研究
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摘要
烟草行业一直是我国财政税收的主力军,发展低危害卷烟产品是烟草行业的工作重点。芳香胺是卷烟烟气中的有害成分,其中1—氨基萘、2—氨基萘、3—氨基联苯、4—氨基联苯已被列为需管制与披露的烟草成份。因此,建立一种简单、有效、准确可靠的卷烟烟气中有害芳香胺的分析方法,客观准确地对卷烟产品中有害芳香胺的释放量进行评价,是一项有意义的工作。
据国外报道,多氟酰化衍生-气相色谱(GC)-选择离子监测(SIM)-质谱(MS)测定主流烟气中芳香胺都取得了较好的效果,在重复这项工作时,我们发现由于涉及提取、衍生、纯化和仪器测定等多个操作过程,要得到准确稳定的测定结果并不容易。因此本文详细地考察了多氟酰化衍生—GC—SIM—MS方法中,萃取方式、萃取次数、萃取液浓度、萃取时间、萃取温度、PH值、氢氧化钠浓度、酰化剂种类、酰化剂用量、酰化温度、酰化时间、三甲胺用量、洗脱剂用量等因素对分离检测的影响,在优化的实验条件下,15min内可实现4种芳香胺的分离检测。1-萘胺、2-萘胺、3-氨基联苯、4-氨基联苯的检测限分别为0.12、0.09、0.13、0.10ng/L,相对标准偏差在3.21%～4.7%之间;标准回收率在93.72%～104.22%之间,此方法用于卷烟主流烟气中几种芳香胺的测定,结果令人满意。
我们还初步探索了最新的方法:直接碘取代衍生—GC—SIM—MS方法测定烟气中的芳香胺。结果表明:直接碘代法操作简单,反应不需无水介质,四个芳香胺的碘代产物分离良好。进一步考察该方法的相关系数、重复性、回收率和检测限后,有望发展成为一种简单、有效的烟气中芳香胺的检测方法。
Tobacco industry has been supported our government finance income. The industry focuses on the development of low harmful cigarette. Aromatic amines have been classified as carcinogens, found in tobacco smoke, in particularly 1-naphthylamine, 2- naphthylamine, 3-Aminobipheny, and 4-Aminobipheny. Therefore, it is highly desirable to establish a simple and efficient method for the trace determination of aromatic amines in tobacco smoke, to assess the safety of tobacco by the amount released of aromatic amine from tobacco smoke.
It is reported that aromatic amines in tobacco smoke were derivatized as pentafluoropropionamides and measured by gas chromatography/mass spectrometry in the selected-ion-monitoring mode, which was a sensitive and accurate method. Re-examining the procedure, we found that it is not easy to get good determination of aromatic amines in tobacco smoke, due to involving many process, such as extration, derivatization, purification and control of GC-MS. Therefore, we investigated the influence of diverse parameters on the extraction and the derivatization process of aromatic amines in tobacco smoke, including the extraction mode, extraction time, extraction temperature, concentration of HCl solution, concentration of sodium hydroxide solution, pH value, derivative reagent kind , derivative temperature , derivative time, amount of derivative reagent and elution solution. Under the optimized conditions, aromatic amines could be separated and detected within 15 min. The detection limits of 3-aminobiphenyl, 4-aminobiphenyl, 1-naphthylamine, 2-naphthylamine are 0.13, 0.10, 0.12, 0.09 ng/L. The recoveries of aromatic amines ranged from 93.72 % to 104.22%. The relative standard derivations ranged from 3.21 % to 4.7 %. This method was applied to the determination of trace aromatic amines in main-stream smoke with good result. In addition, nuclear iodination has been examined preliminary, in this work as an alternative derivatization reaction. Iodination is a relatively moderate process, albeit, it is not subjected to side-reactions and not restricted to anhydrous media. After further investigation of correlation coefficient, limit of detection, relative standard deviations, and the recoveries of aromatic amines by the use of the nuclear iodination, and a promising method will be established, which is sample and efficient one for the trace determination of aromatic amines in tobacco smoke
据国外报道,多氟酰化衍生-气相色谱(GC)-选择离子监测(SIM)-质谱(MS)测定主流烟气中芳香胺都取得了较好的效果,在重复这项工作时,我们发现由于涉及提取、衍生、纯化和仪器测定等多个操作过程,要得到准确稳定的测定结果并不容易。因此本文详细地考察了多氟酰化衍生—GC—SIM—MS方法中,萃取方式、萃取次数、萃取液浓度、萃取时间、萃取温度、PH值、氢氧化钠浓度、酰化剂种类、酰化剂用量、酰化温度、酰化时间、三甲胺用量、洗脱剂用量等因素对分离检测的影响,在优化的实验条件下,15min内可实现4种芳香胺的分离检测。1-萘胺、2-萘胺、3-氨基联苯、4-氨基联苯的检测限分别为0.12、0.09、0.13、0.10ng/L,相对标准偏差在3.21%～4.7%之间;标准回收率在93.72%～104.22%之间,此方法用于卷烟主流烟气中几种芳香胺的测定,结果令人满意。
我们还初步探索了最新的方法:直接碘取代衍生—GC—SIM—MS方法测定烟气中的芳香胺。结果表明:直接碘代法操作简单,反应不需无水介质,四个芳香胺的碘代产物分离良好。进一步考察该方法的相关系数、重复性、回收率和检测限后,有望发展成为一种简单、有效的烟气中芳香胺的检测方法。
Tobacco industry has been supported our government finance income. The industry focuses on the development of low harmful cigarette. Aromatic amines have been classified as carcinogens, found in tobacco smoke, in particularly 1-naphthylamine, 2- naphthylamine, 3-Aminobipheny, and 4-Aminobipheny. Therefore, it is highly desirable to establish a simple and efficient method for the trace determination of aromatic amines in tobacco smoke, to assess the safety of tobacco by the amount released of aromatic amine from tobacco smoke.
It is reported that aromatic amines in tobacco smoke were derivatized as pentafluoropropionamides and measured by gas chromatography/mass spectrometry in the selected-ion-monitoring mode, which was a sensitive and accurate method. Re-examining the procedure, we found that it is not easy to get good determination of aromatic amines in tobacco smoke, due to involving many process, such as extration, derivatization, purification and control of GC-MS. Therefore, we investigated the influence of diverse parameters on the extraction and the derivatization process of aromatic amines in tobacco smoke, including the extraction mode, extraction time, extraction temperature, concentration of HCl solution, concentration of sodium hydroxide solution, pH value, derivative reagent kind , derivative temperature , derivative time, amount of derivative reagent and elution solution. Under the optimized conditions, aromatic amines could be separated and detected within 15 min. The detection limits of 3-aminobiphenyl, 4-aminobiphenyl, 1-naphthylamine, 2-naphthylamine are 0.13, 0.10, 0.12, 0.09 ng/L. The recoveries of aromatic amines ranged from 93.72 % to 104.22%. The relative standard derivations ranged from 3.21 % to 4.7 %. This method was applied to the determination of trace aromatic amines in main-stream smoke with good result. In addition, nuclear iodination has been examined preliminary, in this work as an alternative derivatization reaction. Iodination is a relatively moderate process, albeit, it is not subjected to side-reactions and not restricted to anhydrous media. After further investigation of correlation coefficient, limit of detection, relative standard deviations, and the recoveries of aromatic amines by the use of the nuclear iodination, and a promising method will be established, which is sample and efficient one for the trace determination of aromatic amines in tobacco smoke
引文
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