色谱

色谱 ›› 2013, Vol. 31 ›› Issue (10): 989-994.DOI: 10.3724/SP.J.1123.2013.04005

• 研究论文 • 上一篇    下一篇

液液萃取-气相色谱-质谱联用法同时检测烟用水基胶中的23种酯类化合物

龚淑果, 孔波, 庹苏行, 戴云辉, 吴名剑, 谭立权, 刘巍   

  1. 湖南中烟工业有限责任公司技术研发中心, 湖南 长沙 410007
  • 收稿日期:2013-04-08 修回日期:2013-05-18 出版日期:2013-10-28 发布日期:2013-10-08
  • 通讯作者: 刘巍
  • 基金资助:

    湖南中烟工业有限责任公司基金项目(2012-JC-0004).

Simultaneous determination of 23 ester compounds in cigarette water-borne adhesives by liquid-liquid extraction and gas chromatography-mass spectrometry

GONG Shuguo, KONG Bo, TUO Suxing, DAI Yunhui, WU Mingjian, TAN Liquan, LIU Wei   

  1. Technology Research & Development Center, Hunan Branch of China Tobacco Industrial Corporation, Changsha 410007, China
  • Received:2013-04-08 Revised:2013-05-18 Online:2013-10-28 Published:2013-10-08

PDF

277

被引次数

19

摘要：

建立了一种同时检测烟用水基胶中23种酯类化合物的液液萃取-气相色谱-质谱联用方法。23种酯类化合物包括乙酸酯类、丙烯酸酯类、甲基丙烯酸酯类、邻苯二甲酸酯类化合物。水基胶样品经水分散后,用含内标物丙酸苯乙酯的正己烷溶液振荡萃取,萃取液离心后过0.45 μm有机相滤膜,用DB-WAXETR气相色谱柱(60 m×0.25 mm×0.25 μm)分离,质谱选择离子模式监测,内标法定量。结果表明,23种酯类化合物在0.4~50.0 mg/L范围内线性关系良好,线性相关系数大于0.998,样品加标回收率为81.8%~109.1%,相对标准偏差(RSD, n=5)小于4%,检出限为0.02~0.76 mg/kg,定量限为0.04~2.52 mg/kg。该方法前处理简便、快速、分析时间短、灵敏度高、重复性好,可用于烟用水基胶中23种酯类化合物的同时检测。

关键词: 气相色谱-质谱联用法, 烟用水基胶, 液液萃取, 酯类化合物

Abstract:

A method of gas chromatography-mass spectrometry (GC-MS) with liquid-liquid extraction has been developed for the simultaneous determination of 23 ester compounds including acetate esters, acrylic esters, metacrylic acid esters and phthalate acid esters in cigarette water-borne adhesives. After dispersed in water, the sample was extracted by n-hexane solution containing phenyl ethyl propionate as internal standard substance. Then, the solution was centrifuged and filtrated through a 0.45 μm organic membrane filter. Finally, the solution was separated on a DB-WAXETR column (60 m×0.25 mm×0.25 μm), and detected with MS in selected ion monitoring mode, and quantified by internal standard method. The results showed a good linear correlation in the range of 0.4-50.0 mg/L. The recoveries of the ester compounds spiked in the sample were 81.8%-109.1%, and the relative standard deviations (RSDs, n=5) were less than 4%. The limits of detection (LODs) and limits of quantification (LOQs) were in the ranges of 0.02-0.76 mg/kg and 0.04-2.52 mg/kg, respectively. The method is simple, time-saving, and has high sensitivity and good reproducibility. It can be applied to the determination of the 23 ester compounds in cigarette water-borne adhesives.

Key words: cigarette water-borne adhesives, ester compounds, gas chromatography-mass spectrometry (GC-MS), liquid-liquid extraction

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