超高效液相色谱法测定卷烟主流烟气中的7种酚类物质  

Determination of Seven Phenols in Main Stream Smoke of Cigarette by Ultra Performance Liquid Chromatography

作　　者：许永 孔维松 王晋 黄海涛 刘欣 李雪梅 杨叶昆 向明 田丽梅 李晶 XU Yong;KONG Wei-song;WANG Jin;HUANG Haitao;LIU Xin;LI Xuemei;YANG Yekun;XIANG Ming;TIAN Limei;LI Jing(Technology Center of China Tobacco Yunnan Industrial Co.,Ltd.,Kunming,Yunnan 650106)

机构地区：[1]云南中烟工业有限责任公司技术中心,云南昆明650106

出　　处：《安徽农业科学》2018年第11期157-160,共4页Journal of Anhui Agricultural Sciences

基　　金：中国烟草总公司重大专项(110201601034)

摘　　要：[目的]采用超高效液相色谱法测定卷烟主流烟气中的7种酚类物质。[方法]卷烟主流烟气中的酚类用剑桥滤片捕集,然后用自主设计的新型样品前处理装置以1%乙酸超声提取,萃取液采用ACQUITY UPLC BEH C_(18)色谱柱(50 mm×2.1 mm,1.7μm)分离,以1%乙酸(内含0.01 mol/Lβ-CD)和70%乙腈(内含1%乙酸和0.01 mol/Lβ-CD)为流动相进行梯度洗脱,卷烟主流烟气中的主要7种酚类物质在5.0 min内可达到基线分离。[结果]采用新的样品前处理装置可以有效简化前处理步骤,提高分析效率;7种酚类物质在浓度为0.02~25.00μg/mL时具有较好的线性关系,线性相关系数>0.999 00;检出限为2.5~6.5μg/L;在不同添加水平下,平均回收率为93.8%~98.5%,日内精密度和日间精密度考察均小于5%,具有较好的重复性。[结论]该方法能较好地应用于卷烟主流烟气中7种酚类物质的测定。[Objective]The determination of seven phenols in main stream smoke by ultra high performance chromatography was studied.[Method]The phenols were collected by Cambridge filter and extracted from Cambridge filter with 1%acetic acid solution by ultrasonic extraction in self-designed sample pretreatment device.Thereafter,the phenols were separated on an ACQUITY UPLC BEH C 18(50 mm×2.1 mm,1.7μm)rapid column taking 1%acetic acid solution(containing 0.01 mol/Lβ-CD)and 70%acetonitrile(containing 1%acetic acid and 0.01 mol/Lβ-CD)as mobile phase by gradient elution.The seven phenols can be separated completely within 5.0 min.[Result]The pretreatment steps can be simplified with self designed sample pretreatment device.The 7 analytes could be separated smoothly with good linearity in the range of 0.02-25.00μg/mL,with the correlation coefficients larger than 0.999 00.The limits of detection(LODs)were further evaluated(2.5-6.5μg/L).The mean recovery of the target compounds was 93.8%-98.5%for 7 phenols and the intra-day and inter-day precision were below 5%.[Conclusion]This method was applied to the determination of phenols in main stream smoke with satisfactory results.

关 键 词：卷烟 主流烟气 酚类 超高效液相色谱法(UPLC) 新型前处理装置 

分 类 号：O657.72[理学—分析化学] TS411[理学—化学]