超声辅助离子液体分散液液微萃取-高效液相色谱法测定蜂蜜中的咖啡因  

Determination of caffeine in honey by ultrasound-assisted ionic liquid based dispersive liquid-liquid microextraction coupled with high performance liquid chromatography

作　　者：于玲[1] 董丽丽[1] 

机构地区：[1]邢台学院化学工程与生物技术学院,河北邢台054001

出　　处：《中国卫生检验杂志》2015年第23期4027-4030,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立超声辅助离子液体分散液液微萃取样品前处理技术,结合高效液相色谱测定蜂蜜中咖啡因的方法。方法样品采用分散固相萃取吸附剂N-丙基乙二胺(PSA)、C18、石墨炭黑粉(GCB)净化后,用离子液体[Omim][PF6]做萃取剂,甲醇做分散剂,通过超声、离心、对目标物进行富集,用高效液相色谱-紫外检测器分析测定,同时对分散固相萃取吸附剂的选择及影响分散液液微萃取的因素进行了优化。结果在最优条件下,咖啡因的富集倍数达到120倍,检出限为0.2μg/L,线性范围为1μg/L^500μg/L,线性相关系数为0.999 6,平均加标回收率为84.1%~108.5%,相对标准偏差(RSD)为2.4%~3.7%。结论方法具有简便快速、准确灵敏、萃取效率高、有机溶剂消耗少等特点。建立的方法能成功用于蜂蜜中咖啡因的测定。Objective A method for the determination of caffeine in honey was developed by pretreatment of dispersive solid phase extraction and ultrasound-assisted dispersive liquid-liquid microextraction coupled with high performance liquid chromatography. Methods The sample was purified by primary secondary amine（ PSA）,C18 and graphitized carbon black（ GCB）powder. With ionic liquid as extraction solvents and methanol as disperser solvents,the sample was determined by high performance liquid chromatography（ HPLC） after ultrasound and centrifugation. The sorbent selection and the important parameters that affected the extraction efficiency were optimized. Results Under the optimum conditions,the enrichment factors of caffeine was about 120 times. The limits of detection was 0. 2 μg / L,and the linearity ranges were among 1 μg / L-500 μg / L,with the correlation coefficient of 0. 999 6. The average recoveries ranged from 84. 1% to 108. 5%,and the relative standard deviation（ RSD） was among 2. 5%-4. 7%. Conclusion With the advantages of simplicity,accuracy,high extraction efficiency and little consumption,this method can be successfully applied for the determination of caffeine in honey.

关 键 词：分散固相萃取 分散液液微萃取 高效液相色谱法 咖啡因 蜂蜜 

分 类 号：O657.72[理学—分析化学]