食品科学 ›› 2019, Vol. 40 ›› Issue (20): 318-324.doi: 10.7506/spkx1002-6630-20181120-227

• 安全检测 • 上一篇    下一篇

可可碱、茶碱和咖啡碱的快速测定及其色谱保留行为

聂吉语,李荣,王颖,汤书华,谭津,包荣,姜子涛   

  1. (1.天津商业大学生物技术与食品科学学院,天津市食品生物技术重点实验室,天津 300134;2.天津天狮学院食品工程学院,天津 301700)
  • 出版日期:2019-10-25 发布日期:2019-10-25
  • 基金资助:
    天津市自然科学基金项目(16JCYBJC43300;17JCQNJC02400)

NIE Jiyu, LI Rong, WANG Ying, TANG Shuhua, TAN Jin, BAO Rong, JIANG Zitao

NIE Jiyu, LI Rong, WANG Ying, TANG Shuhua, TAN Jin, BAO Rong, JIANG Zitao   

  1. (1. Tianjin Key Laboratory of Food Biotechnology, School of Biotechnology and Food Science, Tianjin University of Commerce, Tianjin 300134, China; 2. School of Food Engineering, Tianjin Tianshi College, Tianjin 301700, China)
  • Online:2019-10-25 Published:2019-10-25

摘要: 建立基于钛胶反相色谱固定相快速测定食品中可可碱、茶碱和咖啡碱的高效液相色谱(high performance liquid chromatography,HPLC)法。结果表明,可可碱、茶碱和咖啡碱的标准曲线线性良好(R2>0.999 0),线性范围分别为5~500、5~1 000 mg/mL和6~1 200 mg/mL,检出限分别为0.04、0.08 mg/mL和0.03 mg/mL,样品加标回收率分别为99.0%~102.0%、96.7%~106.7%和99.4%~102.3%,相对标准偏差(n=9)小于0.23%。3 种生物碱在HPLC上的保留行为由焓变ΔH0驱动,保留顺序与实验结果相符,依次为可可碱、茶碱和咖啡碱。建立方法操作简单、分析速度快,精密度和准确度均可满足测定要求。用于食品中可可碱、茶碱和咖啡碱的同时测定,结果满意。

关键词: 钛胶反相色谱柱, 高效液相色谱法, 热力学, 可可碱, 茶碱, 咖啡碱

Abstract: A rapid method for simultaneous determination of the contents of theobromine, theophylline and caffeine in beverages by high performance liquid chromatography (HPLC) with a titania-based reverse-phase column was developed. The proposed method presented good linearity (R2 > 0.999 0) for theobromine, theophylline and caffeine in the range of 5–500, 5–1 000 and 6–1 200 mg/mL, respectively, under the optimum?conditions, and the limits of detection (LODs) for them were 0.04, 0.08 and 0.03 mg/mL, respectively. The recoveries of spiked samples were 99.0%–102.0%, 96.7%–106.7% and 99.4%–102.3%, respectively. The relative standard deviations (RSDs) of the precision for 9 replicate detections were less than 0.23%. This method was simple in operation and fast in analysis. Both the precision and accuracy could meet the requirements of quantitative analysis.?The method could be used for simultaneous determination of theobromine, theophylline and theobromine in food, giving satisfactory results. In addition, the thermodynamic parameters, entropy, enthalpy and Gibbs free energy, were calculated for the retention of the analytes. The retention behaviors of the three alkaloids were driven by enthalpy change ΔH0, and the retention sequence of theobromine, theophylline and theobromine was consistent with the experimental results.

Key words: titania-based reverse phase column, high performance liquid chromatography, thermodynamics, theobromine, theophylline, caffeine

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