顶空-程序升温气化-气相色谱-氮化学发光检测器/质谱法测定雪茄烟叶中13种碱性香味化合物的含量  

Determination of 13 Alkaline Aromatic Compounds in Cigar Tobacco Leaves by Gas Chromatography-Nitrogen Chemiluminescence Detector/Mass Spectrometry with Headspace-Programmable Temperature Vaporizing

作　　者：李俊杰 周妍 焦亮[1] 戚大伟[1] 费婷[1] 吴达[1] 刘百战[1] LI Junjie;ZHOU Yan;JIAO Liang;QI Dawei;FEI Ting;WU Da;LIU Baizhan(Technical Center,Shanghai Tobacco Group Co.,Ltd.,Shanghai 201315,China)

机构地区：[1]上海烟草集团有限责任公司技术中心,上海201315

出　　处：《理化检验（化学分册）》2024年第11期1085-1092,共8页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：中国烟草总公司科技重点项目(110202201033 XJ-04)。

摘　　要：提出了顶空-程序升温气化-气相色谱-氮化学发光检测器/质谱法(HS-PTV-GC-NCD/MS)测定雪茄烟叶中13种碱性香味化合物含量的方法,并与美国国家标准与技术研究院(NIST)质谱库匹配,鉴定出39种碱性香味化合物。雪茄烟叶于40℃烘干10 h,研磨过80目(0.178 mm)筛,取过筛后的烟末样品0.5 g置于15 mL离心管中,加入含5%(质量分数)氢氧化钠的饱和氯化钠溶液5 mL和20.0 mg·L^(-1)乙醇胺内标溶液20μL,于25℃振荡萃取0.5 h,以转速4500 r·min^(-1)离心10 min,取上清液过0.45μm水相滤膜,取2 mL滤液置于20 mL顶空瓶中,在DB-WAX色谱柱上按照柱升温程序分离,NCD定量分析。结果表明,13种碱性香味化合物的质量浓度在一定范围内与对应的NCD峰面积与内标的NCD峰面积比呈线性关系,检出限(3S/N)为0.60~2.99μg·kg^(-1);按照标准加入法进行回收试验,回收率为72.0%~103%,日内和日间测定值的相对标准偏差(n=5)均小于10%;方法用于分析不同产地的雪茄烟叶样品,13种碱性香味化合物均被检出,检出量为0.9~5050.4μg·kg^(-1)。A method for determination of 13 alkaline aromatic compounds in cigar tobacco leaves by gas chromatographynitrogen chemiluminescence detector/mass spectrometry with headspace-programmable temperature vaporizing(HS-PTV-GCNCD/MS)was proposed,and 39 alkaline aromatic compounds were identified,by matching with the mass spectrometry library of the National Institute of Standards and Technology(NIST)in the United States.Cigar tobacco leaves were dried at 40℃for 10 h,ground,and passed through a 80 mesh(0.178 mm)sieve.0.5 g of the sieved tobacco powder sample was taken and placed in a 15 mL-centrifuge tube.5 mL of saturated sodium chloride solution containing 5%(mass fraction)sodium hydroxide and 20μL of 20.0 mg·L^(−1) ethanolamine internal standard solution were added.The solution was extracted by shaking at 25℃for 0.5 h,and centrifuged at a rotational speed of 4500 r·min^(−1) for 10 min.The supernatant was passed through a 0.45μm water phase filter membrane,and 2 mL of the filtrate was placed in a 20 mL-headspace flask.Targets in the solution was separated on a DB-WAX chromatographic column according to the column heating program,and NCD was used for quantitative analysis.As shown by the results,linear relationships between the ratios of the corresponding NCD peak area to the internal standard NCD peak area and mass concentrations of 13 alkaline aromatic compounds were found in definite ranges,with detection limits(3S/N)in the range of 0.60-2.99μg·kg−1.Test for recovery was made by the standard addition method,giving results in the range of 72.0%-103%,with RSDs(n=5)of the determined values of intra-day and inter-day less than 10%.This method was used for the analysis of cigar tobacco leaf samples from different origins,and 13 alkaline aromatic compounds were all detected,with detection amounts in the range of 0.9-5050.4μg·kg−1.

关 键 词：顶空-程序升温气化 气相色谱法 氮化学发光检测器 质谱法 雪茄烟叶 碱性香味化合物 

分 类 号：O657.63[理学—分析化学]