Determination of 5 Phenyl Ethyl Carboxylates in Cut Tobacco by GC-MS/MS with Accelerated Solvent Extraction and Evaluation on Uniformity Evalution of the Aromatizing Process
摘 要
将烟丝样品置于温度(20±1)℃及相对湿度(60±3)%条件下平衡24 h。称取此样品4.0 g置于Dionex ASE 350萃取仪的34 mL萃取池中,用正己烷作为溶剂进行加速溶剂萃取(ASE)。加速萃取的温度为100℃,静态萃取时间为5 min,循环次数为2次。于萃取液中加入乙酸苯甲酯内标(100 mg·L-1)溶液0.50 mL,混匀后经0.45 μm滤膜过滤,取滤液进行气相色谱-串联质谱法分析。采用HP-5MS毛细管色谱柱(30 m×0.25 mm,0.25 μm),在60~280℃温度区间程序升温模式分离后,按电子轰击离子源和多反应监测模式条件进行串联质谱测定。所测定的5种羧酸苯乙酯的质量浓度均在0.10~10.00 mg·L-1内与其对应的峰面积之间呈线性关系,其检出限(3S/N)均为0.01 mg·L-1。按标准加入法测定了方法的回收率,结果为91.0%~107%,测定值的相对标准偏差(n=6)均小于10%。同一批次内和不同批次间外加标记物的变异系数(CVi)分别为5.8%~8.8%和6.3%~8.4%,说明加香工序的均匀性良好。
Abstract
Cut tobacco sample was equilibrated for 24 h under the condition of (20±1)℃ and relative humidity of (60±3)%. A portion (4.0 g) of the equilibrated sample was taken and transferred to the 34 mL of extraction cell of the Dionex ASE 350 extractor and submitted to ASE with n-hexane. In ASE process, conditions of temperature (100℃), static extraction time (5 min), and cycling frequency (2 times) were adopted. The extract was separated and 0.50 mL of 100 mg·L-1 phenylmethyl acetate solution was added as internal standard. After well mixing and filtration through 0.45 μm filtering membrane, the filtrate was used for GC-MS/MS analysis. Chromatographic separation was carried out on HP-5MS capillary column (30 m×0.25 mm, 0.25 μm) and under the mode of programmed temperature elevation ranged from 60℃ to 280℃. EI and MRM mode were used in MS/MS determination. Linearily ranges of standard curves of the 5 phenylethyl carboxylates determined were found same between 0.10 mg·L-1 and 10.00 mg·L-1, and their detection limits (3S/N) were found having the same value of 0.01 mg·L-1. Recovery was tested by standard addition method, and the results of recovery were found in the range of 91.0%-107%, and values of RSDs (n=6) were found all less than 10%. Uniformity of aromatizing process for the cut tobacco were tested on samples taken from intra and inter production batches of the aromatizing process, giving values of coefficients of variation (CVi) in the ranges of 5.8%-8.8% and 6.3%-8.4%, respectively, showing that the uniformity of aromatizing was good and satifactory.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202001002
所属栏目 试验与研究
基金项目 上海烟草集团有限责任公司科技项目(K2018-2-013P)
收稿日期 2019/5/17
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备注吴若昕,助理工程师,硕士,主要从事化学分析、烟草化学工作
引用该论文: WU Ruoxin,ZHANG Chuntao,LI Dengke,ZHANG Xiaoli,ZHANG Jianzhong,LI Haixia. Determination of 5 Phenyl Ethyl Carboxylates in Cut Tobacco by GC-MS/MS with Accelerated Solvent Extraction and Evaluation on Uniformity Evalution of the Aromatizing Process[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(1): 7~13
吴若昕,张春涛,李登科,张小利,张建中,李海霞. 加速溶剂萃取-气相色谱-串联质谱法测定烟丝中5种羧酸苯乙酯的含量及对烟丝加香的均匀性评价[J]. 理化检验-化学分册, 2020, 56(1): 7~13
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参考文献
【1】廖惠云,张映,熊晓敏,等.基于标志物含量的变化表征卷烟制丝加香均匀性[J].烟草科技, 2011(10):5-11.
【2】廖惠云,张映,郝喜良.卷烟制丝加料工序均匀性的评价与控制[J].烟草科技, 2008(8):5-7.
【3】刘泽,何邦华,陈林,等.基于料液施加效果的加料工序关键工艺参数优化[J].烟草科技, 2015(4):71-75.
【4】陈闯,张尚明,许宗保,等.一种基于木糖醇检测白肋烟处理加料均匀性评价方法:201210172531.X[P]. 2012-09-19.
【5】鹿洪亮,舒芳誉,罗志雪,等.一种卷烟加香均匀性评价方法:200910112579.X[P]. 2011-04-27.
【6】王文领,马宇平,赵志伟,等.评价卷烟加香均匀性的方法[J].烟草科技, 2003(9):19-22.
【7】夏启东,何邦华,侯英,等.气相色谱质谱法测定6种加香目标物质的含量及对烟丝加香均匀性的评价[J].分析测试学报, 2012,31(7):816-822.
【8】刘泽春,黄华发,洪伟龄,等.过程能力分析在卷烟加料均匀性评价中的应用[J].烟草科技, 2010,10:5-7.
【9】于宏晓,徐海涛,马强,等.电子鼻气味指纹数据对烟丝加香质量的评价[J].中国烟草科学, 2010,31(2):63-66.
【10】汪显国,申晓锋,刘泽,等.基于主成分分析法的烟丝加香均匀性评价[J].中国烟草学报, 2013,19(5):33-42.
【11】申进朝.复杂植物样品分析中的样品处理技术与应用研究[D].合肥:中国科学技术大学, 2006.
【12】欧小群,马丽艳,潘赛超,等.加速溶剂萃取技术在食品安全检测中的应用[J].中国食品学报, 2018,18(5):222-231.
【13】陈玲,李剑政,杨文彬.应用加速溶剂萃取法分离烟丝致香成分[J].分析测试学报, 2007,26(S1):296-299.
【2】廖惠云,张映,郝喜良.卷烟制丝加料工序均匀性的评价与控制[J].烟草科技, 2008(8):5-7.
【3】刘泽,何邦华,陈林,等.基于料液施加效果的加料工序关键工艺参数优化[J].烟草科技, 2015(4):71-75.
【4】陈闯,张尚明,许宗保,等.一种基于木糖醇检测白肋烟处理加料均匀性评价方法:201210172531.X[P]. 2012-09-19.
【5】鹿洪亮,舒芳誉,罗志雪,等.一种卷烟加香均匀性评价方法:200910112579.X[P]. 2011-04-27.
【6】王文领,马宇平,赵志伟,等.评价卷烟加香均匀性的方法[J].烟草科技, 2003(9):19-22.
【7】夏启东,何邦华,侯英,等.气相色谱质谱法测定6种加香目标物质的含量及对烟丝加香均匀性的评价[J].分析测试学报, 2012,31(7):816-822.
【8】刘泽春,黄华发,洪伟龄,等.过程能力分析在卷烟加料均匀性评价中的应用[J].烟草科技, 2010,10:5-7.
【9】于宏晓,徐海涛,马强,等.电子鼻气味指纹数据对烟丝加香质量的评价[J].中国烟草科学, 2010,31(2):63-66.
【10】汪显国,申晓锋,刘泽,等.基于主成分分析法的烟丝加香均匀性评价[J].中国烟草学报, 2013,19(5):33-42.
【11】申进朝.复杂植物样品分析中的样品处理技术与应用研究[D].合肥:中国科学技术大学, 2006.
【12】欧小群,马丽艳,潘赛超,等.加速溶剂萃取技术在食品安全检测中的应用[J].中国食品学报, 2018,18(5):222-231.
【13】陈玲,李剑政,杨文彬.应用加速溶剂萃取法分离烟丝致香成分[J].分析测试学报, 2007,26(S1):296-299.
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