Determination of Caffeine in Honey by HPLC Coupled with Ultrasound-Assisted Dispersive Liquid-Liquid Microextraction
摘 要
采用超声辅助分散液相微萃取技术结合高效液相色谱法测定蜂蜜中的咖啡因.将样品用水溶解配制成100 g·L-1样品溶液,取7.5 mL样品溶液,加入三氯甲烷120 μL和甲醇1.5 mL,混匀后超声5 min,离心后吸取5 μL沉积相,在WondasilTM C18色谱柱上分离,以甲醇(1+1)溶液为流动相进行洗脱,紫外检测波长为274 nm.咖啡因的线性范围为10.0~500 μg·L-1,检出限(3S/N)为9 μg·L-1.测定值的相对标准偏差为2.7%~4.1%,加标回收率在96.6%~104%之间.
Abstract
A method of HPLC combined with ultrasound-assisted dispersive liquid-liquid microextraction was used for the determination of caffeine in honey.The honey sample was dissolved in water to a mass concentration of 500 g·L-1.7.5 mL of the solution was mixed with 150 μL of chloroform and 1.5 mL of methanol by ultrasound for 5 min.The mixture was centrifuged.5 μL of the sedimentary phase was separated on a WondasilTM C18 column using methanol (1+1) solution as the mobile phase for elution.UV detection was made at the wavelength of 274 nm.The linearity range of caffeine was 10.0-500 μg·L-1 with detection limit (3S/N) of 9 μg·L-1.The recovery rates measured by standard addition method ranged from 96.6% to 104%,and the RSD ranged from 2.7% to 4.1%.
中图分类号 O652.63 DOI 10.11973/lhjy-hx201507002
所属栏目 试验与研究
基金项目
收稿日期 2014/6/9
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备注于玲(1983-),女,河北宁晋人,讲师,研究方向为色谱在食品、药品分析中的应用.
引用该论文: YU Ling,DONG Li-li,WANG Xiu-ling,HU Zhang-ji,LI Min,WANG Jun-chun. Determination of Caffeine in Honey by HPLC Coupled with Ultrasound-Assisted Dispersive Liquid-Liquid Microextraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(7): 897~901
于玲,董丽丽,王秀玲,胡章记,李敏,王俊春. 超声辅助分散液相微萃取-高效液相色谱法测定蜂蜜中的咖啡因[J]. 理化检验-化学分册, 2015, 51(7): 897~901
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参考文献
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【19】臧晓欢,吴秋华,张美月,等.分散液相微萃取技术研究进展[J].分析化学,2009,37(2):161-168.
【20】熊芳,李拥军,戴华.蜂蜜中咖啡因含量的液相色谱法测定[J].分析测试学报,2002,21(5):97-99.
【2】KRETSCHMAR J A,BAUMANN T W.Caffeine in citrus flowers[J].Phytochemistry,1999,52(1):19-23.
【3】El-SHAHAWI M S,HAMZA A,BAHAFFI S O,et al.Analysis of some selected catechins and caffeine in green tea by high performance liquid chromatography[J].Food Chemistry,2012,134(4):2268-2275.
【4】ROSTAGNO M A,MANCHN M.D′Arrigo,et al.Fast and simultaneous determination of phenolic compounds and caffeine in teas,mate,instant coffee,soft drink and energetic drink by high-performance liquid chromatography using a fused-core column[J].Analytica Chimica Acta,2010,685(2):204-211.
【5】GUO Su-juan,ZHU Qian-qian,YANG Bao-cheng,et al.Determination of caffeine content in tea based on poly (safranine T) electroactive film modified electrode[J].Food Chemistry,2011,129(3):1311-1314.
【6】NISHITANI E,SAGESAKA Y M.Simultaneous determination of catechins,caffeine and other phenolic compounds in tea using new HPLC method[J].Journal of Food Composition and Analysis,2003,17(5):675-685.
【7】李琛,陈悦鸣,李迎丽.反相高效液相色谱法测定茶饮料中儿茶素类化合物和咖啡因[J].理化检验-化学分册,2011,47(9):1080-1085.
【8】SN/T 1354-2004进出口蜂蜜中咖啡因含量检验方法[S].
【9】REZAEE M,ASSADI Y,Mohammad-Reza Milani Hosseini,et al.Determination of organic compounds in water using dispersive liquid-liquid microextraction[J].Journal of Chromatography A,2006,1116(1/2):1-9.
【10】BERIJANI S,ASSADI Y,ANBIA M,et al.Dispersive liquid-liquid microextraction combined with gas chromatography-flame photometric detection[J].Journal of Chromatography A,2006,1123(1):1-9.
【11】SHI Zhi-hong,YAN Jun-jing,MA Shi-pan.Dispersive liquid-liquid microextraction based on solidification of floation organic droplet for HPLC determination of tanshinones in traditional chinese medicinal injections containing salvia miltiorrhiza bunge[J].Journal of Liquid Chromatography and Related Technologies,2013,36(15):2095-2106.
【12】HAN Dan-dan,TANG Bao-kun,ROW K H.Determination of diuretic drugs in human urine using dispersive liquid-liquid microextraction by high performance liquid chromatography[J].Journal of Liquid Chromatography & Related Technologies,2013,36(15):2069-2081.
【13】叶朝霞,李莉,胡文凌,等.分散液相微萃取-高效液相色谱法测定水和土壤中多环芳烃[J].理化检验-化学分册,2012,48(4):467-470.
【14】MALEKI R,FARHADI K,NIKKHAHI Y.Trace determination of malachite green in water samples using dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography-diode array detection[J].International Journal of Environmental Analytical Chemistry,2012,92(9):1026-1035.
【15】ZHOU Shu,WU Bo,MA Chao,et al.Solid-phase extraction followed by dispersive liquid-liquid microextraction for the sensitive determination of carbamates in environmental water by high-performance liquid chromatography[J].Journal of Liquid Chromatography and Related Technologies,2012,35(20):2860-2872.
【16】LIU Zhi-mei,LIU Wei-hua,RAO Huan,et al.Determination of some carbamate pesticides in watermelon and tomato samples by dispersive liquid-liquid microextraction combined with high performance liquid chromatography[J].International Journal of Environmental Analytical Chemistry,2012,92(5):571-581.
【17】沈英,孙福生,董杰.分散液相微萃取-高效液相色谱法测定水中丙溴磷农药[J].分析化学,2010,38(4):551-554.
【18】LI Yan-yan,WEI Guo-hui,HU Jia,et al.Dispersive liquid-liquid microextraction followed by reversed phase-high performance liquid chromatography for the determination of polybrominated diphenyl ethers at trace levels in landfill leachate and environmental water samples[J].Analytica Chimica Acta,2008,615(1):96-103.
【19】臧晓欢,吴秋华,张美月,等.分散液相微萃取技术研究进展[J].分析化学,2009,37(2):161-168.
【20】熊芳,李拥军,戴华.蜂蜜中咖啡因含量的液相色谱法测定[J].分析测试学报,2002,21(5):97-99.
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