气质联用测定卷烟主流烟气中的3-羟基吡啶

摘要

[目的]研究卷烟主流烟气粒相物中3-羟基吡啶含量,为卷烟感官评吸提供参考.[方法]采用N-甲基-N-三甲基硅烷三氟乙酰胺(MSTFA)-气相色谱-质谱分析化学手段,建立了3-羟基吡啶快速、高效、可靠的分析方法.该方法是用剑桥滤片采集卷烟烟气粒相物加内标(苯酚-D5)后用三氯甲烷进行超声萃取,衍生化后的萃取液进行气相色谱-质谱联用(GC-MS)分析.[结果]3-羟基吡啶衍生物能在较短时间内出峰,色谱峰型较好,检出限(3S/N)为31 ng/支,加标回收率在97.3%~98.1%,测定值的相对标准偏差(n=6)在1.5%~2.9%.[结论]该方法适用于卷烟主流烟气中3-羟基吡啶的快速分析.%[Objective] To study the content of pyridin-3-ol in the particulate phase of mainstream cigarette smoke and provide reference for cigarette sensory evaluation.[Method] A rapid, efficient and reliable method for the determination of pyridin-3-ol was established by adopting N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) Silanization-GC-MS.The method is to use the Cambridge filter collection cigarette smoke particulate and adding internal standard (Phenol-D5) after extracted ultrasonically with chloroform, derivatization and extraction liquid after GC-MS analysis.[Result] The results showed that: The pyridin-3-ol derivatives can be produced in a short period of time, good chromatographic peak type, detection limit (3S/N) of the method found was 31 ng/cig, values of recovery found by standard addition method were in the range of 97.3%-98.1%, and values of RSD's (n=6) were found in the range of 1.5%-2.9%.[Conclusion] This method is suitable for the rapid analysis of pyridin-3-ol in mainstream cigarette smoke.