GC-MS/MS法结合多元统计过程控制应用于烟用香精的质量监控  

GC-MS/MS combining with multivariate statistical process control for quality monitoring of tobacco flavor

作　　者：蒋成勇[1] 杜国荣[1] 王丽达 张杰[1] 严莉红 白若石[1] 郑晓曼[1] 芦楠[1] 周骏[1] JIANG Chengyong;DU Guorong;WANG Lida;ZHANG Jie;YAN Lihong;BAI Ruoshi;ZHENG Xiaoman;LU Nan;ZHOU Jun(Beijing Working Station,Technology Center of Shanghai Tobacco Group Co.,Ltd.,Beijing 101121,China)

机构地区：[1]上海烟草集团有限责任公司技术中心北京工作站

出　　处：《烟草科技》2019年第8期44-51,共8页Tobacco Science & Technology

基　　金：上海烟草集团有限责任公司科技项目“烟用香精的质量控制方法研究及其在卷烟产品质量监控中的应用”（K2017-2-014P）

摘　　要：为利用香气成分监控烟用香精质量,建立了同时测定烟用香精中全组分香气成分的气相色谱-串联质谱法(GC-MS/MS),并结合多元统计过程控制(MSPC)建立了烟用香精质量监控模型。以丙酮为溶剂,料液比为1∶20,超声提取5min,提取液静置过滤后用DB-WAX柱分离,在多反应监测(MRM)模式下测定,采用内标校正法进行半定量分析。通过基于主成分分析(PCA)的MSPC技术并结合感官评价,计算统计量HotellingT2,以3σ为控制上限绘制控制图,对烟用香精进行质量评价。结果表明:大多数香气成分的检出限小于1.0ng/mL,加标回收率为80%~120%,日内和日间重复性(RSD)分别小于3%和5%。该方法灵敏度高,准确性好;基于全组分香气成分分析建立的质量监控模型从客观上反映了烟用香精的内在质量波动,适用于烟用香精质量的快速、准确判定。To monitor the quality of tobacco flavor via aroma components, a GC-MS/MS(gas chromatographytandem mass spectrometry) method was established for simultaneously determining all aroma components in tobacco flavors. Furthermore, a quality monitoring model for tobacco flavors was developed on the basis of MSPC(multivariate statistical process control). The flavor samples were separated on a DB-WAX column after extracted with acetone at the sample/solvent ratio of 1∶20 and ultrasonic extraction time of 5 min. The extracts were analyzed by GC-MS/MS under the multi-reaction monitoring(MRM) mode, and internal standard correction method was applied to semi-quantify aroma components. Statistic Hotelling T^2 was calculated by a PCA-based MSPC method combining with the sensory evaluation of cigarettes, and a control chart was drawn by taking 3σ as the upper control limit to assess the quality of tobacco flavors. The results showed that the LODs of the most aroma components were less than1.0 ng/mL, the recoveries ranged from 80% to 120% with the intra-and inter-day relative standard deviations(RSDs)less than 3% and 5% respectively. This method features a high sensitivity and good accuracy. The quality monitoring model based on the analysis of all aroma components objectively reflects the intrinsic quality fluctuation of tobacco flavors and is suitable for the rapid and accurate evaluation of tobacco flavor quality.

关 键 词：GC-MS/MS 多元统计过程控制 烟用香精 质量监控 

分 类 号：TS4[农业科学—烟草工业] S572