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为简化样品前处理操作步骤,减小分析误差,设计了一种带有柱层析净化功能的索氏提取装置,基于该装置建立了测定卷烟主流烟气中苯并[a]芘(B[a]P)释放量的索氏提取-气相色谱-质谱(GC/MS)方法,并采用该方法对肯塔基参比卷烟2R4F和14个不同类型的卷烟样品进行了测定。结果表明:1利用该装置可直接对捕集卷烟主流烟气总粒相物后的剑桥滤片进行提取、净化和浓缩,浓缩液用GC/MS在选择离子监测模式下进行测定。2方法的线性范围为5~500 ng/mL(R~2=0.999 5),B[a]P的加标回收率为95.4%~104.2%,平均相对标准偏差(RSD)2.32%,检测限0.12 ng/支。32R4F参比卷烟和14个不同类型卷烟样品主流烟气中B[a]P的测定结果与采用GB/T 21130—2007方法的测定结果基本一致。该方法操作简便,灵敏度和准确度较高,适用于卷烟主流烟气中B[a]P的测定。
In order to simplify the operation steps of sample pretreatment and reduce the analysis error, a Soxhlet extraction device with column chromatography purification function was designed. Based on this device, the determination of benzo [a] pyrene (B [ A] P release was determined by Soxhlet extraction-gas chromatography-mass spectrometry (GC / MS). The Kentucky reference cigarette 2R4F and 14 different types of cigarette samples were determined by this method. The results show that: 1 The device can be used directly to capture the mainstream tobacco cigarette smoke after the total particulate matter of the Cambridge filter extraction, purification and concentration, concentrated liquid GC / MS in selected ion monitoring mode was measured. The linear range of the method was 5 ~ 500 ng / mL (R ~ 2 = 0.999 5). The spiked recoveries of B [a] P ranged from 95.4% to 104.2% with an average relative standard deviation (RSD) of 2.32% 0.12 ng / branch. The determination results of B [a] P in mainstream smoke of 32R4F reference cigarette and 14 different types of cigarettes samples are in good agreement with those obtained by the method of GB / T 21130-2007. The method is simple, sensitive and accurate, and is suitable for the determination of B [a] P in cigarette mainstream smoke.