色谱

色谱 ›› 2012, Vol. 30 ›› Issue (03): 298-303.DOI: 10.3724/SP.J.1123.2011.11014

• 研究论文 • 上一篇    下一篇

高效液相色谱-蒸发光散射检测法在烟用香精料液中水溶性糖及山梨醇分析中的应用

胡斌*, 王昇, 谢复炜, 刘惠民   

  1. 中国烟草总公司郑州烟草研究院, 河南 郑州 450001
  • 收稿日期:2011-11-08 修回日期:2011-12-21 出版日期:2012-03-28 发布日期:2012-05-02
  • 通讯作者: 胡斌,博士,高级工程师,主要从事烟草化学、农药残留分析等领域的研究. Tel: (0371)67672738,
  • 基金资助:

    国家烟草专卖局科技攻关项目(No.110200601026).

Application of high performance liquid chromatography-evaporative light scattering detection in determination of water-soluble sugars and sorbitol in tobacco flavourings and casings

HU Bin*, WANG Sheng, XIE Fuwei, LIU Huimin   

  1. Zhengzhou Tobacco Research Institute of China National Tobacco Corporation, Zhengzhou 450001, China
  • Received:2011-11-08 Revised:2011-12-21 Online:2012-03-28 Published:2012-05-02

PDF

347

被引次数

23

摘要：

建立了高效液相色谱-蒸发光散射(HPLC-ELSD)同时检测烟用香精料液中6种水溶性糖及山梨醇的分析方法。方法选用Isolute ENV+固相萃取(SPE)小柱净化样品提取液,以Prevail Carbohydrate ES高效糖柱(250 mm×4.6 mm, 5 μm)作为分析柱,以乙腈和水(75:25, v/v)作为流动相,在1.0 mL/min流速下实现目标物的良好分离;蒸发光散射检测器漂移管温度为79 ℃,载气流速为2.0 L/min。方法针对各目标物建立双对数工作曲线,线性范围约为0.06～1.2 g/L,检出限为12～26 mg/L,样品加标回收率为88%～109%。针对蒸发光散射检测器的双对数工作曲线,通过实验进行分析对比,并结合前人的工作,指出目标物的物理化学性质及其在色谱柱上的保留状态和流动相的洗脱能力等都是影响检测信号的因素。

关键词: 高效液相色谱, 山梨醇, 双对数工作曲线, 水溶性糖, 烟用香精料液, 蒸发光散射检测

Abstract:

A simultaneous determination method of water-soluble sugars (rhamnose, xylose, fructose, glucose, sucrose, maltose) and sorbitol in tobacco flavourings and casings based on high performance liquid chromatography-evaporative light-scattering detection (HPLC-ELSD) was established. The analytes were extracted with ultrasonic assisted extraction into water and cleaned-up by Isolute ENV+solid phase extraction (SPE) cartridge, and then separated on Prevail Carbohydrate ES column (250 mm×4.6 mm, 5 μm) with acetonitrile and water (75:25, v/v) as mobile phase. The temperature of the drift tube in ELSD was 79 ℃ and the flow rate of carrier gas of nitrogen was 2.0 L/min. The calibration curves were plotted on the double logarithmic scales with the mass concentrations of analytes in the range of about 0.06~1.2 g/L. The limits of detection (LODs) were in the range of 12~26 mg/L. And the spiked recoveries in real samples were 88%~109%. Based on the double logarithmic calibration of analytes, experiments were carried out to indicate that the physical and chemical characteristics of analytes, the retention behaviors on column and the elution ability of mobile phase can all influence the response of ELSD.

Key words: double logarithmic calibration curve, evaporative light-scattering detection (ELSD), sorbitol, tobacco flavourings and casings, water-soluble sugar, high performance liquid chromatography (HPLC)