分散固相萃取-GC-MS/MS法同时检测卷烟主流烟气中21种酰胺类化合物  

Simultaneous determination of 21 amides in mainstream cigarette smoke by gas chromatography-tandem mass spectrometry combined with dispersive solid phase extraction

作　　者：潘立宁[1] 刘瑞红 秦亚琼[1] 王晓瑜[1] 王冰[1] 陈满堂 郭军伟[1] 崔华鹏[1] 余晶晶[1] 樊美娟[1] 刘绍锋[1] PAN Lining;LIU Ruihong;QIN Yaqiong;WANG Xiaoyu;WANG Bing;CHEN Mantang;GUO Junwei;CUI Huapeng;YU Jingjing;FAN Meijuan;LIU Shaofeng(Zhengzhou Tobacco Research Institute of CNTC,Zhengzhou 450001,China)

机构地区：[1]中国烟草总公司郑州烟草研究院,郑州450001

出　　处：《烟草科技》2023年第6期48-58,共11页Tobacco Science & Technology

基　　金：郑州烟草研究院院长科技发展基金项目“气相色谱-串联质谱联用法检测卷烟烟气中酰胺类化合物”(342018CA0210);2021年烟草行业烟草化学重点实验室B类创新平台专项项目(312021AW0420);中国烟草总公司科技重点研发项目“烤烟烟叶风格与质量的化学表征组学研究”(110202002003)。

摘　　要：为研究卷烟主流烟气中与感官相关的酰胺成分,基于分散固相萃取技术结合GC-MS/MS同时测定卷烟主流烟气中21种酰胺类化合物。通过优化提取、净化、色谱分离和质谱多反应监测等关键前处理条件和仪器参数,建立了酰胺类化合物的分析方法;对12个不同品牌和不同焦油释放量的市售卷烟进行测试,研究了卷烟烟气中21种酰胺类化合物的释放量水平及其影响因素。结果表明:①选择石墨化炭黑作为分散固相萃取吸附剂,烟气基质净化效果好、21种酰胺类化合物的回收率高,所建分析方法灵敏度高、准确性好、抗基质干扰能力强。②酰胺类化合物沸点较高,在卷烟主流烟气中主要分布于粒相物中。③卷烟样品中可检出其中的16种酰胺类化合物,释放量范围为0.4~303.9 ng/mg(以平均单位TPM释放量计);其余5种未检出。④12种酰胺类化合物的释放量与TPM高度正相关(相关系数大于0.8)。⑤T检验结果显示,7种酰胺类化合物在混合型卷烟中单位TPM释放量与烤烟型卷烟有极显著性或显著性差异,混合型卷烟明显高于烤烟型卷烟。To study the sensory-related amide components in cigarette smoke,21 amide compounds in mainstream cigarette smoke were determined by gas chromatography-tandem mass spectrometry combined with dispersive solid phase extraction.The analytical method for amides was developed after optimization of key pre-treatment conditions and instrumental parameters,such as extraction,purification,chromatographic separation and multi-reaction monitoring of mass spectrometry.Twelve commercial cigarette samples of different brands with different tar yields were tested for their releases of the 21 amides in mainstream smoke and the influencing factors.The results showed that:1)Graphitized carbon black was selected as the adsorbent for dispersive solid phase extraction due to its better purification effect for cigarette smoke matrix and higher recoveries for the 21 amides,and the established analytical method had higher sensitivity,better accuracy,and stronger anti-interference ability.2)Due to their higher boiling points,the amides were mainly distributed in the particulate matter of mainstream smoke.3)Among them,sixteen amides were detected in cigarette samples with a release range of 0.4-303.9 ng/mg(normalized to average release per mass unit TPM),and the remaining five amides were not detected.4)The releases of 12 amides were highly positively correlated with TPM,with the correlation coefficient being higher than 0.8.5)T-test results indicated that the releases(normalized to per mass unit TPM)of 7 amides from blended type of cigarettes were significantly higher than those from Virginia type cigarettes.

关 键 词：卷烟 主流烟气 酰胺类化合物 分散固相萃取 气相色谱-串联质谱 感官相关成分 

分 类 号：TS411.2[农业科学—烟草工业]