烟草及烟气中部分成分的定量分析
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摘要
研究烟草及烟气中的成分,对烟草行业减害降焦和增香保润等工作具有指导意义。本文主要利用超高效液相色谱法对烟草中的三种主要多酚类物质、苯并[α]芘以及烟气中的七种简单酚进行定量分析,利用超高效液相色谱-电喷雾串联质谱法对烟草及烟气中的烟草特有亚硝胺行定量分析,具体研究内容如下：
(1)建立了超高效液相色谱-二极管阵列检测器同时快速测定烟丝中的绿原酸、芸香苷和莨菪亭的方法。分别采用了两种处理方法：①以1%的醋酸水溶液作溶剂超声萃取烟丝,经0.2μm滤膜过滤后直接进行超高效液相色谱分析。相对标准偏差为2.6‰～4.6%,回收率为85.8%～91.7%。②利用微波辅助提取烟丝,通过单因素试验和正交试验确定最佳提取条件：以体积分数为60%的甲醇水溶液为提取剂、萃取液温度为94℃,微波时间1 min、料液比1:20(g/mL)。方法回收率在96.5%-109.6%之间,相对标准偏差小于5%。与超声提取相比,微波辅助提取有效缩短提取时间,效率更高,重现性好,适合批量卷烟烟丝样品多酚的快速检测。
(2)建立了快速测定主流烟气中(邻、间、对)-苯二酚、(邻、间、对)甲酚和苯酚的超高效液相色谱荧光检测法。采用1%的醋酸水溶液对剑桥滤片进行超声萃取后,经0.2 u m滤膜过滤直接进行超高效液相色谱分析。利用荧光检测器分别对七种简单酚进行定性定量,且(间、对)-甲酚可以完全分开。利用本法检测卷烟主流烟气中简单酚相对标准偏差为0.7‰～4.6%,回收率为86.6%～96.9%。该法具有前处理简便、分析时间短、重现性好等优点,适合卷烟主流烟气中酚类物质的批量快速检测。
(3)建立了烟丝中苯并[α]芘残留的超高效液相色谱荧光检测法。将烟末用环已烷超声提取40 min后过滤,滤液旋蒸浓缩至十,再用甲醇-丙酮(V甲醇：V丙酮=10:1)重新溶解于容量瓶中,经0.2 u m的滤膜过滤后检测。苯并[α]芘在浓度为0.43-43.20 ng/mL范围内呈线性,相关系数为0.9998。样品回收率在94.9%～101.0%之间,相对标准偏差为3.2%。方法检测限为0.11 ng/g,定量限为0.37 ng/g。结果表明本法前处理简便、检测限低、灵敏度高,适用于烟丝中苯并[α]芘分析。
(4)首次建立了超高效液相色谱-电喷雾串联质谱法准确快速测定卷烟主流烟气及烟丝中4种烟草特有亚硝胺的方法。对前处理方法及部分液相条件进行了系统的对比分析,实验结果表明：①由于NNK、NNN、NAB、NAT性质不完全相同,经固相萃取柱纯化无法得到对4个烟草特有亚硝胺回收率都较好的洗脱方法,同时用两个氘代内标对4个烟草特有亚硝胺定量会有偏差,因此采用含4个氘代内标的萃取液萃取后经固相萃取柱纯化直接检测的方法,结果更为准确。②分别采用不同pH值的溶剂作萃取液,发现其检测结果的相对标准偏差小于4.7%,说明萃取液pH值对萃取效果影响很小。③不同柱温对NNN、NAT色谱峰形有影响,相对高的柱温能消除NNN及NAT的分叉峰,但分叉峰的出现并不影响定量的准确性。④NNK、NNN、NAB、NAT的检出限分别为0.10、0.26、0.22、0,08ng/mL,烟丝中TSNAs的回收率92.4%～99.4%,烟气中TSNAs的回收率101.7%～107.5%,检测的相对标准偏差小于10%。本方法适用于卷烟样品主流烟气及烟丝中烟草特有亚硝胺的快速分析。
The investigation of the harmful components in cut tobacco and smoke is one of main task in tobacco industry.Tish is helpful for increasing aroma and reducing harm of cigarettes. In this work, the determination methods for three major polyphenols, benzo[a]pyrene, tobacco-specific nitrosamines (TSNAs) and seven volatile phenols were developed based on ultra-high performance liquid chromategraphy (UPLC) and ultra-high performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-ESI-MS/MS). The results of this study are as follows:
(1) A fast method based on ultra-performance liquid chromatography-photodiode array detector (UPLC-PDA) was developed for determination of scopoletin, chlorogenicacid and rutin in cut tobacco simultaneously.①The cut tobacco were extracted with 1% acetic acid water solution under ultrasonic, the extract was detected by UPLC-PDA after flitting with 0.2μm filter membrane. The polyphenols were quantified by PDA. The results showed that the RSD%(Relative standard derive) of determination of polyphenols in cut tobacco were 2.6%-4.6% with recoveries were 85.8%-91.7%.②The extraction of copoletin, chlorogenicacid and rutin in cut tobacco with microwave-assisted extraction was studied.The optimal extraction conditions of polyphenols were determined by single-factor and the orthogonal experience. The optimal conditions were as follows:methol concentration was 70%, extraction solvent temperature was 94℃,microwave extraction time was 1 min and solid to liquid ratio was 120(g/mL). The recoveries of polyphenols in cut tobacco were 96.5%-109.6%, the RSD% were lower then 5%. The effect of microwave-assisted extraction was obviously more effective compare with ultrasonic extraction. The method has advantage of simply pretreat procedure, lower time-consuming and high reproducibility, it was suitable for the fast analysis of phenolic compounds in cut tobacco.
(2) A method based on ultra performance liquid chromatography with fluorescence detection (UPLC-FLD) was developed for determination of (o, p, m)dihydroxybenzene, (o, p, m)cresol and volatile phenol simultaneously. The Cambridge filter pads (CFPs) were used to collect smokes, then extracted with 1% acetic acid water solution under ultrasonic, the extract was deteced by UPLC-FLD after filtrated with 0.2μm filter membrane. The volatile phenols were quantitated and qualitated by FLD separately, and (m,p)cresol were separated completely. The results showed that the RSD% of determination of volatile phenols in mainstream smoke were 0.7%-4.6% with recoveries were 86.6%-96.9%. The method has advantage of simply pretreated procedure and high precision, it is suitable for the fast analysis of volatile phenols in mainstream smoke.
(3) An accurate and simple method for the determation of Benzo[α] pyrene in cut tobacco based on UPLC-FLD was developed. The samples were extracted with cyclohexane under ultrasonic for 40 min, the extract was concentrated by evaporation plant after filter, then dissolved by menthol and acetone (V/V=10/1) and analyzed by UPLC-FLD. The mobile phase consisted of acetonitrile (85%) and water (15%), The Benzo[a]pyrene was detected at excitation wavelength 365 nm and emission wavelength 410 nm with the flow rate at 0.2 mL/min. The method showed good linearity over the range of 0.43-43.20 ng/mL, the correlation coefficient of linear equation was 0.9998. The recoveries were 94.9%-101.0%with the 3.2% of RSD%. The limit of detection (LOD) and the limit of quantity (LOQ) were 0.11 ng/g and 0.37 ng/g, respectively. This method was suitable for the qualitative and quantitative analysis of Benzo [α] pyrene in cut tobacco, due to its simpleness, sensitivity and high precision.
(4) An accurate and rapid method for the determination of TSNAs in cut tobacco and mainstream smoke was developed based on UPLC-ESI-MS/MS. The pre-treatment procedure and liquid chromatogram conditions for the determination of TSNAs were compared and optimized systematically, the results showed that:Due to the different properties of NNK, NNN, NAB, NAT, no good recoveries rates of TSNAs could be achieved by solid phase extraction (SPE), and all of four TSNAs could not be measured accurately with two deuterated internal standards. The results were more accurate by detecting TSNAs directly after extraction with four deuterated internal standard.②Using 100 mM ammonium acetate,0.1% acetic acid in water and water as the extraction solvent were compared respectively, with less 5% of the RSD%, indicating that pH value had little effect on the extraction.③The column temperature affect both the peak shape of NNN, NAT. High column temperature can eliminate the bifurcation peaks, but tthis does not affect the quantification of TSNAs.④LODs of NNK, NNN, NAB, NAT were 0.10、0.26、0.22、0.08 ng/mL respectively, recoveries of them were 92.4%-99.4% in cut tobacco while were 101.7%-107.5% in mainstream smoke, RSD% were no more than 10%. This method could be used to qualitative and quantitative analysis of TSNAs in both cut tobacco and mainstream smoke.
(1)建立了超高效液相色谱-二极管阵列检测器同时快速测定烟丝中的绿原酸、芸香苷和莨菪亭的方法。分别采用了两种处理方法：①以1%的醋酸水溶液作溶剂超声萃取烟丝,经0.2μm滤膜过滤后直接进行超高效液相色谱分析。相对标准偏差为2.6‰～4.6%,回收率为85.8%～91.7%。②利用微波辅助提取烟丝,通过单因素试验和正交试验确定最佳提取条件：以体积分数为60%的甲醇水溶液为提取剂、萃取液温度为94℃,微波时间1 min、料液比1:20(g/mL)。方法回收率在96.5%-109.6%之间,相对标准偏差小于5%。与超声提取相比,微波辅助提取有效缩短提取时间,效率更高,重现性好,适合批量卷烟烟丝样品多酚的快速检测。
(2)建立了快速测定主流烟气中(邻、间、对)-苯二酚、(邻、间、对)甲酚和苯酚的超高效液相色谱荧光检测法。采用1%的醋酸水溶液对剑桥滤片进行超声萃取后,经0.2 u m滤膜过滤直接进行超高效液相色谱分析。利用荧光检测器分别对七种简单酚进行定性定量,且(间、对)-甲酚可以完全分开。利用本法检测卷烟主流烟气中简单酚相对标准偏差为0.7‰～4.6%,回收率为86.6%～96.9%。该法具有前处理简便、分析时间短、重现性好等优点,适合卷烟主流烟气中酚类物质的批量快速检测。
(3)建立了烟丝中苯并[α]芘残留的超高效液相色谱荧光检测法。将烟末用环已烷超声提取40 min后过滤,滤液旋蒸浓缩至十,再用甲醇-丙酮(V甲醇：V丙酮=10:1)重新溶解于容量瓶中,经0.2 u m的滤膜过滤后检测。苯并[α]芘在浓度为0.43-43.20 ng/mL范围内呈线性,相关系数为0.9998。样品回收率在94.9%～101.0%之间,相对标准偏差为3.2%。方法检测限为0.11 ng/g,定量限为0.37 ng/g。结果表明本法前处理简便、检测限低、灵敏度高,适用于烟丝中苯并[α]芘分析。
(4)首次建立了超高效液相色谱-电喷雾串联质谱法准确快速测定卷烟主流烟气及烟丝中4种烟草特有亚硝胺的方法。对前处理方法及部分液相条件进行了系统的对比分析,实验结果表明：①由于NNK、NNN、NAB、NAT性质不完全相同,经固相萃取柱纯化无法得到对4个烟草特有亚硝胺回收率都较好的洗脱方法,同时用两个氘代内标对4个烟草特有亚硝胺定量会有偏差,因此采用含4个氘代内标的萃取液萃取后经固相萃取柱纯化直接检测的方法,结果更为准确。②分别采用不同pH值的溶剂作萃取液,发现其检测结果的相对标准偏差小于4.7%,说明萃取液pH值对萃取效果影响很小。③不同柱温对NNN、NAT色谱峰形有影响,相对高的柱温能消除NNN及NAT的分叉峰,但分叉峰的出现并不影响定量的准确性。④NNK、NNN、NAB、NAT的检出限分别为0.10、0.26、0.22、0,08ng/mL,烟丝中TSNAs的回收率92.4%～99.4%,烟气中TSNAs的回收率101.7%～107.5%,检测的相对标准偏差小于10%。本方法适用于卷烟样品主流烟气及烟丝中烟草特有亚硝胺的快速分析。
The investigation of the harmful components in cut tobacco and smoke is one of main task in tobacco industry.Tish is helpful for increasing aroma and reducing harm of cigarettes. In this work, the determination methods for three major polyphenols, benzo[a]pyrene, tobacco-specific nitrosamines (TSNAs) and seven volatile phenols were developed based on ultra-high performance liquid chromategraphy (UPLC) and ultra-high performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-ESI-MS/MS). The results of this study are as follows:
(1) A fast method based on ultra-performance liquid chromatography-photodiode array detector (UPLC-PDA) was developed for determination of scopoletin, chlorogenicacid and rutin in cut tobacco simultaneously.①The cut tobacco were extracted with 1% acetic acid water solution under ultrasonic, the extract was detected by UPLC-PDA after flitting with 0.2μm filter membrane. The polyphenols were quantified by PDA. The results showed that the RSD%(Relative standard derive) of determination of polyphenols in cut tobacco were 2.6%-4.6% with recoveries were 85.8%-91.7%.②The extraction of copoletin, chlorogenicacid and rutin in cut tobacco with microwave-assisted extraction was studied.The optimal extraction conditions of polyphenols were determined by single-factor and the orthogonal experience. The optimal conditions were as follows:methol concentration was 70%, extraction solvent temperature was 94℃,microwave extraction time was 1 min and solid to liquid ratio was 120(g/mL). The recoveries of polyphenols in cut tobacco were 96.5%-109.6%, the RSD% were lower then 5%. The effect of microwave-assisted extraction was obviously more effective compare with ultrasonic extraction. The method has advantage of simply pretreat procedure, lower time-consuming and high reproducibility, it was suitable for the fast analysis of phenolic compounds in cut tobacco.
(2) A method based on ultra performance liquid chromatography with fluorescence detection (UPLC-FLD) was developed for determination of (o, p, m)dihydroxybenzene, (o, p, m)cresol and volatile phenol simultaneously. The Cambridge filter pads (CFPs) were used to collect smokes, then extracted with 1% acetic acid water solution under ultrasonic, the extract was deteced by UPLC-FLD after filtrated with 0.2μm filter membrane. The volatile phenols were quantitated and qualitated by FLD separately, and (m,p)cresol were separated completely. The results showed that the RSD% of determination of volatile phenols in mainstream smoke were 0.7%-4.6% with recoveries were 86.6%-96.9%. The method has advantage of simply pretreated procedure and high precision, it is suitable for the fast analysis of volatile phenols in mainstream smoke.
(3) An accurate and simple method for the determation of Benzo[α] pyrene in cut tobacco based on UPLC-FLD was developed. The samples were extracted with cyclohexane under ultrasonic for 40 min, the extract was concentrated by evaporation plant after filter, then dissolved by menthol and acetone (V/V=10/1) and analyzed by UPLC-FLD. The mobile phase consisted of acetonitrile (85%) and water (15%), The Benzo[a]pyrene was detected at excitation wavelength 365 nm and emission wavelength 410 nm with the flow rate at 0.2 mL/min. The method showed good linearity over the range of 0.43-43.20 ng/mL, the correlation coefficient of linear equation was 0.9998. The recoveries were 94.9%-101.0%with the 3.2% of RSD%. The limit of detection (LOD) and the limit of quantity (LOQ) were 0.11 ng/g and 0.37 ng/g, respectively. This method was suitable for the qualitative and quantitative analysis of Benzo [α] pyrene in cut tobacco, due to its simpleness, sensitivity and high precision.
(4) An accurate and rapid method for the determination of TSNAs in cut tobacco and mainstream smoke was developed based on UPLC-ESI-MS/MS. The pre-treatment procedure and liquid chromatogram conditions for the determination of TSNAs were compared and optimized systematically, the results showed that:Due to the different properties of NNK, NNN, NAB, NAT, no good recoveries rates of TSNAs could be achieved by solid phase extraction (SPE), and all of four TSNAs could not be measured accurately with two deuterated internal standards. The results were more accurate by detecting TSNAs directly after extraction with four deuterated internal standard.②Using 100 mM ammonium acetate,0.1% acetic acid in water and water as the extraction solvent were compared respectively, with less 5% of the RSD%, indicating that pH value had little effect on the extraction.③The column temperature affect both the peak shape of NNN, NAT. High column temperature can eliminate the bifurcation peaks, but tthis does not affect the quantification of TSNAs.④LODs of NNK, NNN, NAB, NAT were 0.10、0.26、0.22、0.08 ng/mL respectively, recoveries of them were 92.4%-99.4% in cut tobacco while were 101.7%-107.5% in mainstream smoke, RSD% were no more than 10%. This method could be used to qualitative and quantitative analysis of TSNAs in both cut tobacco and mainstream smoke.
引文
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