液相色谱-串联质谱法测定卷烟主流烟气中的氨基甲酸乙酯  被引量:4

Determination of Ethyl Carbamate in Cigarette Mainstream Smoke by Liquid Chromatography-Tandem Mass Spectrometry

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作  者:朱怀远[1] 庄亚东[1] 刘献军[1] 朱莹[1] 张媛[1] 尤晓娟[1] 张映[1] 熊晓敏[1] 

机构地区:[1]江苏中烟工业有限责任公司技术研发中心,江苏南京210019

出  处:《分析测试学报》2013年第8期963-967,共5页Journal of Instrumental Analysis

基  金:江苏中烟工业有限责任公司科技项目(201201)

摘  要:建立了高效液相色谱-串联质谱法测定卷烟主流烟气中氨基甲酸乙酯含量的分析方法。采用剑桥滤片捕集卷烟主流烟气中的氨基甲酸乙酯,以乙醇为萃取溶剂,振荡技术提取滤片中的目标物,探讨了洗脱溶剂种类、用量及不同类型固相萃取小柱对目标物的净化效果。在优化实验条件下,方法在6~720μg/L范围内具有良好的线性关系,相关系数(r2)为0.999 9,平均加标回收率为93.7%~99.8%,日内重复性RSD小于6%,日间重复性RSD小于5%,定量下限(LOQ)为0.26 ng/cig。该方法准确、灵敏、重现性好、溶剂用量少,适合于卷烟主流烟气中氨基甲酸乙酯含量的测定。An effective liquid chromatography- tandem mass spectrometric (HPLC -MS/MS) meth od was developed for the determination of ethyl carbamate in cigarette mainstream smoke. The ethyl carbamate in cigarette mainstream smoke was trapped with Cambridge filter, and then extracted with an oscillation using ethanol as extraction solvent. Influences of elution solvent type, solvent con sumption and different polarity solid-phase extractions on purification efficiency of the target analyte were discussed. Under the optimal conditions, the calibration curve of the method was in the range of 6 - 720 μg,/with correlation coefficient ( r^2 ) of 0. 999 9. The relative standard deviations (RSDs) of intra-day and inter-day were less than 6% and 5% , respectively. The spiked average recoveries ranged from 93.7% to 99.8% , and the limit of quantitation(LOQ) was 0. 26 ng/cig. With the ad vantages of accurancy, sensitivity, good reproducibility and low solvent consumption, the method was suitable for the determination of ethyl carbamate in cigarette mainstream smoke.

关 键 词:液相色谱-串联质谱法 主流烟气 氨基甲酸乙酯 

分 类 号:O657.63[理学—分析化学] O623.624[理学—化学]

 

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