固相萃取-超高效液相色谱法测定卷烟主流烟气中丙烯酰胺

建立了一种固相萃取-超高效液相色谱法(SPE-UPLC)快速检测主流烟气中丙烯酰胺的方法。使用剑桥滤片和吸收瓶捕集主流烟气后,蒸馏水做萃取溶剂,采用C18固相萃取小柱对样品液进行纯化,用UPLC检测,外标法定量。UPLC方法采用ACQUITY UPLCTMBEH C181.7μm 2.1×50 mm色谱柱,柱温30℃,流动相为V(乙腈)∶V(水)=6∶94,流速为0.15 mL/min,紫外检测器(TUV)检测波长为202 nm,分析时间为6 min。烤烟型香烟主流烟气中丙烯酰胺的含量为4.75μg/cig。方法的线性范围为0.1~10 mg/mL,线性相关系数为0.9999;平均回收率为98.7%;检出限为10 ng/mL(S/N=3);相对标准偏差为2.3%。该方法适合主流烟气中丙烯酰胺的快速检测。

Determination of acrylamide in mainstream cigarette smoke by solid phase extraction-ultra performance liquid chromatography

A new method for rapid determination of acrylamide in mainstream cigarette smoke by SPE-UPLC was developed . After collected in mainstream cigarette smoke by Cambridge filter pad and absorption bottle, the total particulate matte was extracted by distilled water, and purified by solid phase extraction, then detected by UPLC and the quantitative analysis was performed by the external standard method. The optimal experimental conditions were as follows: the column was ACQU1TY UPLC~(TM) BEH C_(18) 1.7 pm 2.1×50 mm column, mobile phase was mixture of acetonitrile and water (6=94, V: V), column temperature was 30 t, TUV detection wavelength was at 202 ran, the analytical time was 6 min. The quantity of acrylamide in flue-cured cigarette mainstream smoke was determined to be 4.75 jug/mL by the method. The calibration curve showed good linearity in the rang of 0.1～10 mg/mL for acrylamind with a correlation coefficient of 0.9999; the average recovery of the method was 98.7%; the detection limit was 10 ng/mL (S/N = 3), RSDwas2.3%. The method was simple, rapid, accurate and well suitable for rapid detection of acrylamide in mainstream cigarette smoke.