Chen Xuan, Li Jie, Hu Shuang, Bai Xiaohong, Zhao Haodong, Zhang Yi
School of Pharmacy, Shanxi Medical University, No. 56, New South Road, Taiyuan 030001, China.
School of Pharmacy, Shanxi Medical University, No. 56, New South Road, Taiyuan 030001, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2018 Jan 1;1072:17-24. doi: 10.1016/j.jchromb.2017.09.023. Epub 2017 Sep 18.
A new fibroin/dodecanol floating solidification microextraction, coupled with high performance liquid chromatography, was developed and applied for enrichment and quantification of the trace flavonoids in traditional Chinese medicine and biological samples. Also, fibroin sensibilization mechanism was described, and influence of sample matrix to enrichment factor was investigated. In this method, a homogeneous fibroin/dodecanol of dispersed solution was employed as microextraction phase to flavonoids (myricetin, quercetin, isorhamnetin, chrysin, kaempferide), the several critical parameters affecting the performance, such as organic extractant, amount of fibroin in organic extractant, volume of extraction phase, dispersant, salt concentration, pH of sample phase, stirring rate, extraction time, and volume of sample phase were tested and optimized. Under the optimized conditions, enrichment factor of flavonoids ranged from 42.4 to 238.1 in different samples, excellent linearities with r≥ 0.9968 for all analytes were achieved, limits of detection were less than or equal to 5.0ng/mL, average recoveries were 92.5% to 115.0% in different samples. The new procedure is simple, fast, low cost, environmentally friendly and high EF, it can also be applied to the concentration and enrichment of the trace flavonoids in other complex matrixes.
一种新型的丝素蛋白/十二醇漂浮固化微萃取技术与高效液相色谱联用,被开发用于富集和定量中药及生物样品中的痕量黄酮类化合物。同时,阐述了丝素蛋白增敏机制,并研究了样品基质对富集因子的影响。在此方法中,以均匀分散的丝素蛋白/十二醇溶液作为黄酮类化合物(杨梅素、槲皮素、异鼠李素、白杨素、山柰酚)的微萃取相,对影响萃取性能的几个关键参数,如有机萃取剂、有机萃取剂中丝素蛋白的量、萃取相体积、分散剂、盐浓度、样品相pH值、搅拌速率、萃取时间和样品相体积进行了测试和优化。在优化条件下,不同样品中黄酮类化合物的富集因子在42.4至238.1之间,所有分析物的线性关系良好,r≥0.9968,检测限小于或等于5.0ng/mL,不同样品中的平均回收率为92.5%至115.0%。该新方法简单、快速、成本低、环境友好且富集因子高,还可应用于其他复杂基质中痕量黄酮类化合物的浓缩和富集。