固相萃取/高效液相色谱法对卷烟主流烟气中丙烯酰胺及其滤咀截留的测定  

Determination of Acrylamide in Mainstream Cigarette Smoke and Cigarette Filter by Solid Phase Extraction/High Performance Liquid Chromatography

作　　者：谢山岭[1,2] 朱瑞芝[1,3] 倪朝敏 向能军 牟定荣 王凯[1,3] 

机构地区：[1]红塔烟草(集团)有限责任公司技术中心,云南玉溪653100 [2]云南大学化学科学与工程学院,云南昆明650091 [3]湖南大学化学化工学院,湖南长沙410082

出　　处：《分析测试学报》2009年第10期1225-1228,共4页Journal of Instrumental Analysis

摘　　要：建立了一种用固相萃取/高效液相色谱法（SPE/HPLC）快速检测主流烟气中丙烯酰胺及其滤咀截留的方法。使用剑桥滤片和吸收瓶捕集主流烟气中的丙烯酰胺,蒸馏水为萃取溶剂,采用C18固相萃取小柱对样品液进行纯化,外标法定量。采用Waters Nova-Pak C18柱（3.9 mm×150 mm×4μm）,柱温30℃,流动相为乙腈-水（体积比3∶47）,流速为0.6 mL/min,DAD检测器检测波长为202 nm对丙烯酰胺进行分离测定,外标法定量。方法的线性范围为0.1-10 mg/L,线性相关系数为0.999 9;回收率为93%-102%,检出限（S/N=3）为0.01 mg/L。测试了8种烤烟型香烟主流烟气中丙烯酰胺的含量为6.89-15.82μg/cig;丙烯酰胺在8种烤烟型香烟滤咀中的截留范围为0.94-1.10μg/cig。A new method was developed for rapid determination of acrylamide in mainstream cigarette smoke and cigarette filter by solid phase extraction/high performance liquid chromatography （SPE/ HPLC）. The mainstream cigarette smoke was collected by Cambridge filter pad and absorption bottle, extracted by distilled water, and purified by solid phase extraction, then detected by HPLC using external standard method for quantification. The optimal conditions was as follows： separation column： Waters Nova-Pak C18 3.9 mm × 150 mm ×4 μm column; column temperature： 30 ℃ ; mobile phase： mixture of acetonitrile and water（3 ： 47, by volume） ; flow rate： 0.6 mL/min; DAD detector： 202 nm. The calibration curve of acrylamide showed a good linearity in the rang of 0. 1 - 10 mg/L with a correlation coefficient of 0. 999 9 and a detection limit（S/N = 3 ） of 0.01 mg/L . The spiked recoveries of the method were between 93% and 102%. The method was used to test the concentration of acrylamide. The result indicated that the amounts of acrylamide in 8 species of fluecured cigarette mainstream and filter samples were in the range of 6. 89 - 15.82 μg/cig and 0.94 - 1.10 μg/eig, respectively.

关 键 词：丙烯酰胺 卷烟 主流烟气 高效液相色谱 

分 类 号：O652.63[理学—分析化学] X795[理学—化学]