固相萃取结合气相色谱-串联质谱法测定烟草制品中23种酯类香料

doi:10.3724/SP.J.1123.2015.12020

色谱 ›› 2016, Vol. 34 ›› Issue (5): 512-519.DOI: 10.3724/SP.J.1123.2015.12020

固相萃取结合气相色谱-串联质谱法测定烟草制品中23种酯类香料

郑阳^1,2, 许秀丽¹, 纪顺利², 袁飞¹, 黄志强³, 杨丙成², 张峰¹

1. 中国检验检疫科学研究院烟草安全与控烟技术中心/食品安全研究所, 北京 100176;
2. 华东理工大学药学院, 上海 200237;
3. 湖南省南检验检疫科学技术研究院, 湖南长沙 410004

收稿日期:2015-12-17 出版日期:2016-05-08 发布日期:2012-12-18
通讯作者: 张峰, 杨丙成
基金资助:
质检公益性行业科研专项(201410088, 201310134);中国检验检疫科学研究院基本科研业务费项目(2016JK009, 2015JK008);国家质检总局科研计划项目(2014IK084);国家重大仪器设备开发专项(2012YQ14000806).

Analysis of 23 esters of flavor additive in tobacco products by gas chromatography-tandem mass spectrometry coupled with solid-phase extraction

ZHENG Yang^1,2, XU Xiuli¹, JI Shunli², YUAN Fei¹, HUANG Zhiqiang³, YANG Bingcheng², ZHANG Feng¹

1. Institute of Tobacco Safety and Control/Institute of Food Safety, Chinese Academy of Inspection and Quarantine, Beijing 100176, China;
2. School of Pharmacy, East China University of Science and Technology, Shanghai 200237, China;
3. Hunan Academy of Science and Technology for Inspection and Quarantine, Changsha 410004, China

Received:2015-12-17 Online:2016-05-08 Published:2012-12-18
Supported by:
Public Welfare Fund of Inspection and Quarantine of China (Nos. 201410088, 201310134); Fund of Chinese Academy of Inspection and Quarantine (Nos. 2016JK009, 2015JK008); Science and Technology Project of Administration of Quality Supervision, Inspection and Quarantine of China (No. 2014IK084); National Key Scientific Instrument and Equipment Development Projects of China (No. 2012YQ14000806).

摘要/Abstract

摘要：

利用固相萃取结合气相色谱-串联质谱(SPE-GC-MS/MS)检测技术建立了烟草制品中23种酯类香料的定量分析方法。样品以乙酸乙酯为提取溶剂,经NH₂固相萃取柱(依次用甲醇和水活化)净化,用4 mL乙酸乙酯洗脱,在多反应监测(MRM)模式下进行检测。结果表明,23种香料在20.0~500.0 μ g/L范围内线性关系良好(r² > 0.996),检出限(LOD, S/N=3)及定量限(LOQ, S/N=10)分别为1.9~13.6 μ g/kg及6.3~45.3 μ g/kg,在1、1.5、2倍定量限的加标水平下,平均回收率为62.1%~91.4%,相对标准偏差(RSD)均小于7%。该方法准确可靠、灵敏度好,适用于烟草制品中23种常用酯类香料的快速筛查与定性、定量分析。该方法为烟草中酯类物质的检测开拓了平台。

关键词: 固相萃取, 气相色谱-串联质谱, 烟草制品, 酯类香料

Abstract:

An analytical method for the simultaneous determination of 23 esters of flavor additive in tobacco products was established based on optimized solid-phase extraction (SPE) with gas chromatography-tandem mass spectrometry (GC-MS/MS). The samples were extracted with ethyl acetate, cleaned up by an amino SPE column. After conditioning step, the extracts were eluted by 4 mL ethyl acetate, and then were determined by GC-MS/MS in multi-reaction monitoring (MRM) mode. The results showed that all the 23 ester flavor additives had good linearity in the range of 20.0-500.0 μ g/L, with the correlation coefficients (r²) better than 0.996. The limits of detection (LODs) and limits of quantitation (LOQs) of these additives were in the ranges of 1.9-13.6 μ g/kg and 6.3-45.3 μ g/kg, respectively. The average recoveries of the 23 analysts were in the range of 62.1%-91.4% at the spiked levels of 1, 1.5, 2 times LOQ with relative standard deviations (RSDs) typically lower than 7%. The accurate, reliable and sensitive method can be applied to the determination of the 23 esters of flavor additive in tobacco products for rapid screening and quantitative analysis. The method also offered an opportunity to detect more ester additives that may be added in tobacco products.

Key words: ester flavor additives, gas chromatography-tandem mass spectrometry (GC-MS/MS), solid phase extraction (SPE), tobacco products

中图分类号:

O658

郑阳, 许秀丽, 纪顺利, 袁飞, 黄志强, 杨丙成, 张峰. 固相萃取结合气相色谱-串联质谱法测定烟草制品中23种酯类香料[J]. 色谱, 2016, 34(5): 512-519.

ZHENG Yang, XU Xiuli, JI Shunli, YUAN Fei, HUANG Zhiqiang, YANG Bingcheng, ZHANG Feng. Analysis of 23 esters of flavor additive in tobacco products by gas chromatography-tandem mass spectrometry coupled with solid-phase extraction[J]. Chinese Journal of Chromatography, 2016, 34(5): 512-519.

参考文献

[1] Carmines E L. Food Chem Toxicol, 2002, 40(1): 77
[2] Baker R R, da Silva J R P, Smith G. Food Chem Toxicol, 2004, 42S: 3S
[3] Marcilla A, Martínez I, Berenguer D, et al. Food Chem Toxicol, 2012, 50(5): 1317
[4] Zheng X Z, Zhang S H, Qiu J Q. Tobacco Science & Technology, 2003(11): 8 郑新章, 张仕华, 邱纪青. 烟草科技, 2003(11): 8
[5] Kong H H, Lu H, Chen C L, et al. Journal of Instrumental Analysis, 2010, 29(6): 612 孔浩辉, 鲁虹, 陈翠玲, 等. 分析测试学报, 2010, 29(6): 612
[6] Hu Y H, Ning M, Zhang X Y, et al. Tobacco Science & Technology, 2015(3): 66 胡永华, 宁敏, 张晓宇, 等. 烟草科技, 2015(3): 66
[7] Dempsey R, Coggins C R E, Roemer E. Regul Toxicol Pharm, 2011, 61(1): 119
[8] Liu Q, Raina A K, Smith M A, et al. Mol Aspects Med, 2003, 24(4): 305
[9] Sepetdjian E, Shihadeh A, Saliba N A. Food Chem Toxicol, 2008, 46(5): 1582
[10] Schubert J, Kappenstein O, Luch A, et al. J Chromatogr A, 2011, 1218: 5628
[11] Chen C, Tian Z, Zhang S M, et al. Acta Tabacaria Sinica, 2014, 20(2): 80 陈闯, 田忠, 张尚明, 等. 中国烟草学报, 2014, 20(2): 80
[12] Hu B B, Wang L, Hu Q, et al. Acta Tabacaria Sinica, 2011, 17(1): 83 胡兵兵, 王黎, 胡群, 等. 中国烟草学报, 2011, 17(1): 83
[13] Guo J. China Measurement and Test, 2012, 38(S1): 50 郭靖. 中国测试, 2012, 38(S1): 50
[14] Dai Y X, Zhu L J, Li H L, et al. Journal of Anhui Agricultural Sciences, 2010, 38(31): 17862 戴迎雪, 朱立军, 黎洪利, 等. 安徽农业科学, 2010, 38(31): 17862
[15] Chen J T, Wang Y L, Zhu G Q. Tobacco Science & Technology, 1993(6): 19 陈建潭, 王以礼, 朱国清. 烟草科技, 1993(6): 19
[16] Lou B, Liu S Y. Journal of Anhui Agricultural Sciences, 2012, 40(29): 14496 娄本, 刘善宇. 安徽农业科学, 2012, 40(29): 14496
[17] Clark T J, Bunch J E. J Agric Food Chem, 1997, 45(3): 844
[18] Zhu X L, Gao Y, Chen Z Y, et al. Chromatographia, 2009, 69(7/8): 735
[19] Li J, Xu J C, Li X M, et al. Chinese Journal of Chromatography, 2012, 30(8): 816 李晶, 徐济仓, 李雪梅, 等. 色谱, 2012, 30(8): 816
[20] Ren Z Q, Ai X Y, Huang Z Q, et al. Chinese Journal of Chromatography, 2015, 33(5): 541 任志芹, 艾小勇, 黄志强, 等. 色谱, 2015, 33(5): 541
[21] Merckel C, Pragst F, Ratzinger A, et al. J Chromatogr A, 2006, 1116(1): 10
[22] Schubert J, Luch A, Schulz T G. Talanta, 2013, 115: 665
[23] Hennion M C. J Chromatogr A, 1999, 856(1): 3
[24] Li G Q, Ma G H. Chinese Journal of Chromatography, 2011, 29(7): 606 李广庆, 马国辉. 色谱, 2011, 29(7): 606
[25] Zheng X H, Lin L Y, Fang E H, et al. Chinese Journal of Chromatography, 2012, 30(1): 27 郑向华, 林立毅, 方恩华, 等. 色谱, 2012, 30(1): 27
[26] Mayr C M, Capone D L, Pardon K H, et al. J Agric Food Chem, 2015, 63(13): 3394
[27] Zhang Y, Wang X J, Li L, et al. J Chromatogr A, 2013, 1306: 72
[28] Shen Y, Hu B, Chen X Z, et al. J Agric Food Chem, 2014, 62(45): 10881
[29] YC/T 31-1996

编辑推荐

Metrics

阅读次数

全文

HTML			PDF

最新录用	在线预览	正式出版	最新录用	在线预览	正式出版
0	0	0	0	0	57

来源	本网站	其他网站

次数	55	2
比例	96%	4%

摘要

最新录用	在线预览	正式出版

0	0	88

	来源	本网站

	次数	88
	比例	100%

固相萃取结合气相色谱-串联质谱法测定烟草制品中23种酯类香料

Analysis of 23 esters of flavor additive in tobacco products by gas chromatography-tandem mass spectrometry coupled with solid-phase extraction

PDF

可视化

被引次数

摘要/Abstract

引用本文

使用本文

扫码分享

参考文献

相关文章 15

编辑推荐

Metrics

[1]	岳超, 赵超群, 毛思浩, 王展华, 施贝, 徐欣丰, 梁晶晶. 通过式固相萃取净化-超高效液相色谱-串联质谱法测定液体乳中10种氨基甲酸酯类农药残留[J]. 色谱, 2023, 41(9): 807-813.
[2]	孟二琼, 念琪循, 李峰, 张秋萍, 许茜, 王春民. 磺酸化磁性氮化碳固相萃取-超高液相色谱-串联质谱筛检淡水鱼中孔雀石绿和隐色孔雀石绿[J]. 色谱, 2023, 41(8): 673-682.
[3]	高祎阳, 丁亚丽, 陈鲁玉, 杜芳, 辛绪波, 冯娟娟, 孙明霞, 冯洋, 孙敏. 共价有机框架材料在固相萃取中的最新应用进展[J]. 色谱, 2023, 41(7): 545-553.
[4]	秦童童, 高莉, 赵文杰. 超交联多孔有机聚合物在柱固相萃取中的应用进展[J]. 色谱, 2023, 41(7): 554-561.
[5]	陈东洋, 张昊, 张磊, 王一红, 王小丹, 冯家力, 梁静, 钟旋. 固相萃取-超高效液相色谱-串联质谱法测定发酵食品中的曲酸[J]. 色谱, 2023, 41(7): 632-639.
[6]	赵原庆, 胡锴, 杨成, 韩鹏昭, 李立新, 刘晓冰, 张振强, 张书胜. 基于Ti₃C₂T_x/聚酰亚胺复合材料的分散固相萃取-液相色谱法测定尿液中儿茶酚胺类神经递质[J]. 色谱, 2023, 41(7): 572-581.
[7]	王秋旭, 冯启言, 朱雪强. 加速溶剂萃取-固相萃取净化结合超高效液相色谱-串联质谱法测定沉积物中双酚类化合物[J]. 色谱, 2023, 41(7): 582-590.
[8]	李洁, 鞠香, 王艳丽, 田其燕, 梁秀清, 李海霞, 刘艳明. QuEChERS-在线凝胶渗透色谱-气相色谱-串联质谱法高通量筛查动物源性食品中的多农药残留[J]. 色谱, 2023, 41(7): 610-621.
[9]	夏宝林, 汪仕韬, 殷晶晶, 张维益, 杨娜, 刘强, 吴海晶. 自动上样固相萃取-超高效液相色谱-串联质谱法同时测定水中9类43种抗菌药物残留[J]. 色谱, 2023, 41(7): 591-601.
[10]	王园媛, 李璐璐, 吕佳, 陈永艳, 张岚. 固相萃取-超高效液相色谱-三重四极杆质谱法测定饮用水中13种卤代苯醌类消毒副产物[J]. 色谱, 2023, 41(6): 482-489.
[11]	宁晓盼, 姚倩, 许忠祥, 殷耀, 柳菡, 张晓燕, 丁涛, 张勇, 侯玉, 王梦茹, 吴丽娜, 汤奇婷. 固相萃取-高效液相色谱法测定水产调味品中7种对羟基苯甲酸酯类防腐剂[J]. 色谱, 2023, 41(6): 513-519.
[12]	李振环, 胡小键, 陆一夫, 谢琳娜, 朱英. 基于高通量全自动固相萃取的超高效液相色谱-串联质谱法测定人尿中16种抗生素和4种β-受体激动剂[J]. 色谱, 2023, 41(5): 397-408.
[13]	宋新力, 王宁, 何飞燕, 程灿玲, 王飞, 王京龙, 张立华. 碳纳米管复合材料结合分散固相萃取-高效液相色谱-串联质谱法检测环境水样中痕量全氟化合物[J]. 色谱, 2023, 41(5): 409-416.
[14]	吴少明, 欧阳立群, 孟鹏, 何孟杭, 林钦, 陈言凯, 刘文菁, 苏晓明, 戴明. 固相萃取净化-超高效液相色谱-串联质谱法测定畜肉中18种卡因类麻醉剂[J]. 色谱, 2023, 41(5): 434-442.
[15]	陆慧媛, 王利娟, 张炯恺, 张驰中, 李天娟, 季瑞雪, 沈伟健. 固相萃取-气相色谱法测定橄榄油中4种脂肪酸乙酯[J]. 色谱, 2023, 41(4): 359-365.