在线固相萃取-气相色谱/热能检测测定卷烟主流烟气中的TSNAs
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摘要
建立了卷烟主流烟气中4种TSNAs的在线固相萃取-气相色谱/热能检测测定方法。在标准吸烟条件下,采用剑桥滤片收集卷烟烟气的总粒相物,滤片经二氯甲烷萃取、过滤后,样品通过固相萃取柱富集,然后切换六通阀用洗脱液反向洗脱下TSNAs,最后进入气相色谱中排干溶剂后通过气相色谱柱分离,用热能检测器检测。结果表明:采用改进后的方法可以简化前处理步骤,4种TSNAs线性范围宽,相关系数均> 0. 999;检出限分别为0. 028 ng/支、0. 020 ng/支、0. 025 ng/支和0. 030 ng/支;在不同添加水平下,平均回收率为94. 2%～102. 8%,日内相对标准偏差和日间相对标准偏差均小于3. 0%。本方法可用于测定卷烟主流烟气中低含量的TSNAs。
A new method for the determination of TSNAs in mainstream cigarette smoke was developed based on gas chromatography with thermal energy analyzer( TEA) and sample preparation with on-line solid phase extraction. Under the standard smoking condition,the total particulate matter( TMP) of mainstream cigarette smoke was trapped by Cambridge filter. Then,the TPM was extracted with dichloromethane and filtered with filter. The filtered samples were enriched by SPE column and eluted in reverse direction. After the solvent transferred into GC had been drained,the TSNAs were separated by gas chromatography and detected with TEA. Our results demonstrated that the optimized method could greatly simplify the sample preparation for GC-TEA analysis. Importantly,TSNAs were separated with good linearity in a wide range. The limits of detection( LODs) were found at 0. 028,0. 020,0. 025 and 0. 030 ng/cig for NNK,NNN,NAB and NAT,respectively. Furthermore,the mean recovery of the target compounds was 94. 2% ～ 102. 8% for the four TSNAs. The intra-day and interday RSDs were both below 3. 0%. This method could be used to quantitative analysis of TSNAs in mainstream cigarette smoke.
A new method for the determination of TSNAs in mainstream cigarette smoke was developed based on gas chromatography with thermal energy analyzer( TEA) and sample preparation with on-line solid phase extraction. Under the standard smoking condition,the total particulate matter( TMP) of mainstream cigarette smoke was trapped by Cambridge filter. Then,the TPM was extracted with dichloromethane and filtered with filter. The filtered samples were enriched by SPE column and eluted in reverse direction. After the solvent transferred into GC had been drained,the TSNAs were separated by gas chromatography and detected with TEA. Our results demonstrated that the optimized method could greatly simplify the sample preparation for GC-TEA analysis. Importantly,TSNAs were separated with good linearity in a wide range. The limits of detection( LODs) were found at 0. 028,0. 020,0. 025 and 0. 030 ng/cig for NNK,NNN,NAB and NAT,respectively. Furthermore,the mean recovery of the target compounds was 94. 2% ～ 102. 8% for the four TSNAs. The intra-day and interday RSDs were both below 3. 0%. This method could be used to quantitative analysis of TSNAs in mainstream cigarette smoke.
引文
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[15] Shimadzu. On-line Pre-processing of Gas Chromatograph-Mass Spectrometer GPC-GCMS/MS.[2018-4-30].https://www. shimadzu. com. cn/an/gcms/prep-q/340. html岛津.在线前处理气相色谱质谱联用仪GPC-GCMS/MS.[2018-4-30]. https://www. shimadzu. com. cn/an/gcms/prep-q/340. html
[2] Hecht SS. J. Natl. Cancer. Inst.,1999,91(14):1194
[3] Burton HR,Dye NK,Bush LP. J. Agric. Food Chem.,1992,40(6):1050
[4] Shang P P,Li X,Nie C,et al. Carcinogenesis,Teratogenesis&Mutagenesis,2012,24(5):340尚平平,李翔,聂聪,等.癌变畸变突变,2012,24(5):340
[5] GB/T 23228-2008. Cigarette-Determination of tobacco specific N-Nitrosamines in total particulate matter of mainstream cigarette smoke-GC-TEA method GB/T 23228-2008.卷烟主流烟气总粒相物中烟草特有N-亚硝胺的测定气相色谱-热能分析联用法
[6] Zhang X,Zhu D L,Han Y,et al. Acta Tab. Sin.,2015,21(3):12张霞,朱东来,韩熠,等.中国烟草学报,2015,21(3):12
[7] Lu Y F,Wu D,Gu W B,et al. J Chin Mass Spectr Soc,2012,33(2):118陆怡峰,吴达,顾文博,等.质谱学报,2012,33(2):118
[8] Gu W B,Zhou W H,Lu Y F,et al. Tobacco Sci. Tech.,2013,10:40顾文博,周宛虹,陆怡峰,等.烟草科技,2013,10:40
[9] Ramirez N,Ozel MZ,Lewis AC,et al. J. Chromatogr. A.,2012(1219):180
[10] Cho Y H,Shin H S. Anal Meth.,2015,7(11):4472
[11] Ding Y,Yang J,Zhu WJ,et al. J. Chin. Chem. Soc-Taip.,2011,58(5):667
[12] Xiong W,Hou H W,Jiang X Y,et al. Anal. Chim. Acta.,2010,674(1):71
[13] Chen X,Jin L F,Liu P P,et al. Tobacco Sci. Tech.,2016,49(3):62陈霞,金立峰,刘萍萍,等.烟草科技,2016,49(3):62
[14] Zhang J,Bai R S,Yang Z D,et al. Tobacco Sci. Tech.,2017,50(2):48张杰,白若石,杨振东,等.烟草科技,2017,50(2):48
[15] Shimadzu. On-line Pre-processing of Gas Chromatograph-Mass Spectrometer GPC-GCMS/MS.[2018-4-30].https://www. shimadzu. com. cn/an/gcms/prep-q/340. html岛津.在线前处理气相色谱质谱联用仪GPC-GCMS/MS.[2018-4-30]. https://www. shimadzu. com. cn/an/gcms/prep-q/340. html