卷烟烟气中性香味成分的半制备HPLC分离与GC-MS测定
Determination of the content of neutral aromatic components from cigarette mainstream smoke by the separation of semi-preparative HPLC and GC-MS
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摘要: 将半制备HPLC分离与GC-MS测定相结合，对某卷烟样品烟气中性香味成分进行分析：先将半制备HPLC分离条件中的馏分收集时间优化为3个时间段，以保证待测化合物在各馏分中不存在交叉.选择离子流色谱图显示，3个馏分中各待测化合物可完全分离，满足定量分析要求.通过建立GC-MS内标标准曲线进行定量分析，结果表明，各组分线性方程相关系数均大于0.999 0，检出限为0.55~13.06μg/kg，定量限为1.85~43.55 μg/kg，说明该方法灵敏度较高.样品测定与回收率实验结果显示，卷烟样品烟气中性香味成分测定平均回收率为64.39%~93.57%，相对标准偏差均小于10%，说明该方法能满足痕量成分定量分析要求，重现性较好.
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关键词:
- 半制备高效液相色谱分离 /
- 气相色谱-质谱联用 /
- 卷烟烟气 /
- 中性香味成分
Abstract: A method for determination of the content of neutral aromatic components from cigarette mainstream smoke by semi-preparative high performance liquid chromatography (semi-preparative HPLC) coupled with gas chromatography-mass spectrometry (GC-MS) was developed:the fraction collection time was determined to three time periods by optimizing the conditions of semi-preparative HPLC in order to ensure that the compounds to be measured don't cross in the fractions. The selected ion chromatogram showed that all target compounds could be separated completely in three fractions and the method could satisfy the demands of quantitative analysis. Quantitative analysis was performed by establishing a GC-MS internal standard curve. The analysis results showed that the correlation coefficients were greater than 0.999 0,the limits of detection (LOD) were 0.55~13.06 μg/kg and the limits of quantitation (LOQ) were 1.85~43.55 μg/kg. It showed that the method has high sensitivity. The results of sample determination and recovery experiment showed that the average added standard recovery of the neutral aromatic components from cigarette mainstream smoke was in the range of 64.39%~93.57% and the relative standard deviations were less than 10%. It showed that the method could satisfy the requirement of quantitative analysis of trace compounds, with good reproducibility. -
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