烟草中几种重要化学成分的分析技术及组分关联性研究
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摘要
当前，反吸烟运动在世界范围内日益高涨。因此，如何提高烟草品质，减少烟草中有害化学成分的含量是烟草科技工作者面临的重要任务。完成这一任务的先决条件之一是开展烟草化学成分的化学及仪器分析技术研究，建立并不断完善影响烟草品质及吸食安全性的相关化学成分含量测定的新分析方法。借助这些分析方法，进行烟草中有害化学成分和烟草香味物质彼此之间的内在关联性研究，进而提出相应的控制措施，使烟草品质得以改善，并为研制“高香气、低危害”的中式卷烟提供强有力的技术支持。为此，本文在广泛的文献调研基础上，开展了下述四个方面的研究工作：
1．建立和完善了利用毛细管气相色谱—氮磷检测器测定烟草特有亚硝胺的分析方法。对烟气捕集条件、萃取时间、层析物质及其它色谱条件进行了优化。该方法消除了以往测定烟草特有亚硝胺分析方法中易出现的前处理乳化现象。方法具有灵敏度较高、重复性较好、无需昂贵的专用检测设备的特点，易于在普通实验室普及，适合烟草生产企业进行烟草及制品品质监控。
2．建立和完善了分光光度法测定烟草中亚硝胺的分析检测方法。首次探讨了烟草中亚硝胺含量与相应烟草系列溶剂萃取物含量的内在联系，研究发现了部分产地烟叶的香气物质与亚硝胺含量的内在规律。我们通过实验可以确定香气物质含量较多的烟叶其亚硝胺含量相对较低，尤其是同等级的云南烟叶比湖南烟叶的香气物质丰富，且其亚硝胺含量相对较少。
3．首次建立了以琼脂为悬浮剂，将悬浮液进样技术和火焰原子吸收分光光度法联用，以标准曲线法和标准加入法相结合测定烟草中钾含量的新分析方法。该方法最突出的优点是烟草样品不需灰化处理，烟草样品粉末与悬浮剂作用直接进样测试，节约了前处理时间和试剂。同时，该方法具有重复性好、准确度高、适合大批量烟草样品分析的特点。
4．首次建立了利用分子印记聚合物压电模拟生物传感器测定烟草中绿原酸含量的新分析方法。该方法所需设备简单，易于实现在线检测，而且该方法具有灵敏度高、重现性好的特点。其回收率为96.7～105.0％，RSD为3.7％，线性范围为5.0×10~(-8)～1.0×10~(-4)mol／L。此外，所用传感器热稳定性和机械稳定性高、制作成本低廉、操作简单。
Today, anti-smoking campaign is springing up around the world. Therefore, how to improve the quality of tobacco products and reduce the contents of harmful substances in tobacco is an important task faced by scientists in tobacco industry. To achieve this, it is vital to study tobacco chemical and instrumental analytical techniques, develop corresponding experimental technology, and set up a series of new analytical method for measurement of those components associated with tobacco quality and its sucking security. With the help of these analytical methods, the relevancy between the contents of harmful components and aroma substances in tobacco could be studied in order to take corresponding controlled action. This will give a fundamental support for us to improve cigarette quality of Chinese style with the character of "high flavor and low harmfulness" . In the present thesis, the following research works were carried out on the basis of extensive literature investigation.1. A method for the determination of tobacco-specific nitrosamines(TSNA) in tobacco smoke using capillary gas chromatography—NPD measurement was developed. A series of experimental conditions, such as smoke substance collection, extraction time, and chromatography substance conditions, were optimised. The new method avoided the phenomenon of emulsification during sample pretreatment, which was often found in past literatures for TSNA determination. The new method has the advantage of high sensitivity, good repeatability and dispensing expensive special equipment. The method will find application in general tobacco laboratory and be suitable for the supervision of tobacco products in tobacco enterprises.2. A spectrophotometric method for the determination of N-nitrosamines in tobacco was developed. The internal relation between the content of N-nitrosamines in tobacco and of corresponding tobacco extractives was investigated, It was shown that aroma substances in tobacco leaf was associated with its N-nitrosamines content in some degree. Our experimental results also indicated that the more the content of aroma substances in tobacco leaf, the less that of nitrosamines. In particular, the content of aroma substances in YunNan tobacco leaf was more ample than that in HuNan tobacco leaf at the same grade, and the content of nitrosamines in YunNan tobacco leaf less than that in HuNan tobacco leaf at the same grade.3. A new analytical method for the determination of potassium in tobacco was
established by the combination of suspention sampling and flame atomic absorption spectrophotometry with agar to be suspending agent for the first time. Standard curve and standard addition methods were applied for the quantitative analysis of potassium in tobacco. The main advantage of this method is that the tobacco powder can be directly injected as suspended sample, and has no need for cineration in advance. In addition, the new method is high repeatable and accurate, and is suitable for the measurement of large quantities of tobacco sample.4. A new method for the determination of chlorogenic acid in tobacco by molecular imprinted polymer modified piezoelectric bio-mimetic sensor was first described. The method is simple in operation, easy to carry out online measurement and its features includes high reproducibility and sensitivity. The method recovery is 96.7-105.0%, RSD 3.7%, and linear range 5.0× 10-8~1.0× 10-4mol/L. Beside, the sensor used in this method is cheap, and with the characteristic of high thermal stability and mechanical stability.
1．建立和完善了利用毛细管气相色谱—氮磷检测器测定烟草特有亚硝胺的分析方法。对烟气捕集条件、萃取时间、层析物质及其它色谱条件进行了优化。该方法消除了以往测定烟草特有亚硝胺分析方法中易出现的前处理乳化现象。方法具有灵敏度较高、重复性较好、无需昂贵的专用检测设备的特点，易于在普通实验室普及，适合烟草生产企业进行烟草及制品品质监控。
2．建立和完善了分光光度法测定烟草中亚硝胺的分析检测方法。首次探讨了烟草中亚硝胺含量与相应烟草系列溶剂萃取物含量的内在联系，研究发现了部分产地烟叶的香气物质与亚硝胺含量的内在规律。我们通过实验可以确定香气物质含量较多的烟叶其亚硝胺含量相对较低，尤其是同等级的云南烟叶比湖南烟叶的香气物质丰富，且其亚硝胺含量相对较少。
3．首次建立了以琼脂为悬浮剂，将悬浮液进样技术和火焰原子吸收分光光度法联用，以标准曲线法和标准加入法相结合测定烟草中钾含量的新分析方法。该方法最突出的优点是烟草样品不需灰化处理，烟草样品粉末与悬浮剂作用直接进样测试，节约了前处理时间和试剂。同时，该方法具有重复性好、准确度高、适合大批量烟草样品分析的特点。
4．首次建立了利用分子印记聚合物压电模拟生物传感器测定烟草中绿原酸含量的新分析方法。该方法所需设备简单，易于实现在线检测，而且该方法具有灵敏度高、重现性好的特点。其回收率为96.7～105.0％，RSD为3.7％，线性范围为5.0×10~(-8)～1.0×10~(-4)mol／L。此外，所用传感器热稳定性和机械稳定性高、制作成本低廉、操作简单。
Today, anti-smoking campaign is springing up around the world. Therefore, how to improve the quality of tobacco products and reduce the contents of harmful substances in tobacco is an important task faced by scientists in tobacco industry. To achieve this, it is vital to study tobacco chemical and instrumental analytical techniques, develop corresponding experimental technology, and set up a series of new analytical method for measurement of those components associated with tobacco quality and its sucking security. With the help of these analytical methods, the relevancy between the contents of harmful components and aroma substances in tobacco could be studied in order to take corresponding controlled action. This will give a fundamental support for us to improve cigarette quality of Chinese style with the character of "high flavor and low harmfulness" . In the present thesis, the following research works were carried out on the basis of extensive literature investigation.1. A method for the determination of tobacco-specific nitrosamines(TSNA) in tobacco smoke using capillary gas chromatography—NPD measurement was developed. A series of experimental conditions, such as smoke substance collection, extraction time, and chromatography substance conditions, were optimised. The new method avoided the phenomenon of emulsification during sample pretreatment, which was often found in past literatures for TSNA determination. The new method has the advantage of high sensitivity, good repeatability and dispensing expensive special equipment. The method will find application in general tobacco laboratory and be suitable for the supervision of tobacco products in tobacco enterprises.2. A spectrophotometric method for the determination of N-nitrosamines in tobacco was developed. The internal relation between the content of N-nitrosamines in tobacco and of corresponding tobacco extractives was investigated, It was shown that aroma substances in tobacco leaf was associated with its N-nitrosamines content in some degree. Our experimental results also indicated that the more the content of aroma substances in tobacco leaf, the less that of nitrosamines. In particular, the content of aroma substances in YunNan tobacco leaf was more ample than that in HuNan tobacco leaf at the same grade, and the content of nitrosamines in YunNan tobacco leaf less than that in HuNan tobacco leaf at the same grade.3. A new analytical method for the determination of potassium in tobacco was
established by the combination of suspention sampling and flame atomic absorption spectrophotometry with agar to be suspending agent for the first time. Standard curve and standard addition methods were applied for the quantitative analysis of potassium in tobacco. The main advantage of this method is that the tobacco powder can be directly injected as suspended sample, and has no need for cineration in advance. In addition, the new method is high repeatable and accurate, and is suitable for the measurement of large quantities of tobacco sample.4. A new method for the determination of chlorogenic acid in tobacco by molecular imprinted polymer modified piezoelectric bio-mimetic sensor was first described. The method is simple in operation, easy to carry out online measurement and its features includes high reproducibility and sensitivity. The method recovery is 96.7-105.0%, RSD 3.7%, and linear range 5.0× 10-8~1.0× 10-4mol/L. Beside, the sensor used in this method is cheap, and with the characteristic of high thermal stability and mechanical stability.
引文
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