气相色谱-质谱联用法同时测定烟用香精香料中18种邻苯二甲酸酯、香豆素及黄樟素

　　

摘要：建立了气相色谱-质谱联用法同时测定香精香料中18种邻苯二甲酸酯（PAEs)、香豆素及黄樟素的检测方法，以乙醇为萃取溶剂、涡旋振荡10 min提取香精香料样品中的PAEs、香豆素及黄樟素。选择DB-5ms毛细管色谱柱分离各化合物，同时采用选择离子监测的模式进行分析，同位素内标法定量，得到20种化合物的线性方程及相关系数，线性相关系数的范围为0.9991～0.9998，方法检出限为0.07～ 0.42 mg·kg^-1，定量限为0.25～1.41mg·kg^-1，各目标化合物的回收率在85.7% ~ 114.5%，相对标准偏差（n=7）小于4.1%。该方法前处理简单、回收率高、重复性好，适用于香精香料中18种PAEs、香豆素及黄樟素的检测需求。

关键词：气相色谱-质谱联用法；邻苯二甲酸酯；香豆素；黄樟素；内标法

中图分类号：O657.63

GC-MS Simultaneous Determination of 18 Phthalates 、Safrole and Coumarin In Tobacco Essence

NIU En-li¹, NI Bo-li¹, MAO Ning¹, YAN Hong-jun², YANG Yu-ming¹, MA Bin¹

(1.Technology Center, GANSU Tobacco Industrial CO., LTD., Lanzhou 730050, China; 2.Cooperation Production office, China Tobacco zhejiang Industrial CO., LTD., Zhejiang Hangzhou 310024)

Abstract: A method of GC-MS was developed for simultaneous determination of 18 phthalates (PAES), safrole and coumarin in tobacco essence, Ethanol was selected as the extraction solvent to extract 18 PAEs , safrole and coumarin in the tobacco essence by vortex oscillation for 10 minutes. The DB-5ms capillary column was choiced to separate all the compounds，at the same time, the SIM mode of decetion was choosed for analysis. Isotope internal standard method was

used for Quantitative analysis , The calibration curves of 20 compounds with correlation coefficients were in the range of 0.9991~0.9998, The limits of detection of the method for target compounds ranged from 0.07 to 0.42 mg·kg^-1, the limits of quantitation varied from 0.25 to 1.41 mg·kg^-1, The recoveries of target compounds ranged from 85.7% to 114.5% with relative standard deviations(RSDs, n=7) was less than 4.1%, This method was well suitable to detect 18 PAEs , safrole and coumarin in tobacco essence with its simple pre-treatment, high recovery rate and good repeatability.

Key words: GC-MS; PAEs; safrole; coumarin ; internal standard

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