中心切割二维液相色谱-串联质谱法测定卷烟主流烟气中4种芳香胺类化合物的含量  

Determination of 4 Aromatic Amines in Mainstream Cigarette Smoke by Heart-Cutting Two Dimensional Liquid Chromatography-Tandem Mass Spectrometry

作　　者：王天南 戚大伟[1] 汪阳忠 陈敏[1] 陶立奇 费婷[1] 吴达[1] 陆捷 WANG Tiannan;QI Dawei;WANG Yangzhong;CHEN Min;TAO Liqi;FEI Ting;WU Da;LU Jie(Technical Center of Shanghai Tobacco Group Co.,Ltd.,Shanghai 201315,China)

机构地区：[1]上海烟草集团有限责任公司技术中心,上海201315

出　　处：《理化检验（化学分册）》2024年第4期349-357,共9页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：提出了中心切割二维液相色谱-串联质谱法(2DLC-MS/MS)测定卷烟主流烟气中1-氨基萘(1-NA)、2-氨基萘(2-NA)、3-氨基联苯(3-ABP)和4-氨基联苯(4-ABP)等4种芳香胺类化合物含量的方法。用剑桥滤片捕集20支卷烟烟气粒相物,加入200μL 1 mg·L^(-1)混合内标溶液和20 mL 5%(质量分数)盐酸溶液,超声萃取30 min。分取10 mL,加入1 mL 50%(质量分数)氢氧化钠溶液调节溶液酸度至pH 7,再加入2 mL二氯甲烷,涡旋振荡15 min,有机相经0.2μm聚四氟乙烯滤膜过滤。第一维液相色谱法采用强阳离子交换(SCX)色谱柱对目标物进行分离除杂,通过补偿泵在线稀释、中和有机相,目标物被保留于捕集柱,随后目标物被洗脱至第二维反相(RP)色谱系统,分离后在质谱检测器的多反应监测(MRM)模式下,采用内标法定量分析。结果表明:1-NA和2-NA标准曲线的线性范围为0.50~50.0μg·L^(-1),3-ABP和4-ABP标准曲线的线性范围为0.25~50.0μg·L^(-1),检出限(3S/N)为0.002~0.008 ng·支^(-1);4种目标物在3个加标浓度水平下的回收率为86.0%~97.4%,日间精密度与日内精密度试验所得测定值的相对标准偏差均小于8.0%。对市售烤烟型和混合型卷烟样品进行分析,所得混合型卷烟烟气芳香胺类化合物的测定值与盒标焦油量呈正相关,而烤烟型卷烟无明显线性关系。A method for the determination of 4 aromatic amines,including 1-amino-naphthalene(1-NA),2-amino-naphthalene(2-NA),3-aminobenzene(3-ABP),4-aminobenzene(4-ABP)in mainstream cigarette smoke by heart-cutting two dimensional liquid chromatography-tandem mass spectrometry(2DLC-MS/MS)was proposed.The particulate matter of 20 cigarettes smoke was collected with Cambridge filter,and 200μL of 1 mg·L^(-1)the mixed internal standard solution and 20 mL of 5%(mass fraction)hydrochloric acid solution were added for ultrasonic extraction for 30 min.An aliquot(10 mL)was taken,and 1 mL of 50%(mass fraction)sodium hydroxide solution was added to adjust the solution adicity to pH 7.Then 2 mL of dichloromethane was added,and the mixed solution was shaken by vortex for 15 min.The organic phase was filtered by 0.2μm polytetrafluoroethylene filter membrane.A strong cation exchange(SCX)column was used in the first dimensional liquid chromatography to separate and remove impurities from the targets,the organic phase was diluted and neutralized online by compensation pump,and targets were retained in the trap column.Then the targets were eluted to the second dimensional reversed phase(RP)chromatography system,and the multiple reaction monitoring(MRM)mode of mass spectrometry detector was used,with internal standard method for quantitative analysis.It was shown that the linear ranges of the standard curves were 0.50-50.0μg·L^(-1)for 1-NA and 2-NA,and 0.25-50.0μg·L^(-1)for 3-ABP and 4-ABP,with detection limits in the range of 0.002-0.008 ng in a cigarette.The recovery of the 4 targets at 3 spiked concentration levels were in the range of 86.0%-97.4%.Tests for precision of intra-day and inter-day were made,with RSDs of determined values less than 8.0%.The samples of commercial Virginia type cigarettes and blended-type cigarettes were analyzed,and the determined value of aromatic amines in blended-type cigarettes presented positive linear relationship with the labeled tar value.No linear relationship was observed for Virginia type cigar

关 键 词：卷烟烟气 芳香胺类化合物 中心切割二维液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学]