摘要
建立了水性化妆品中睾酮、甲基睾酮和孕酮的聚合物整体柱微萃取和高效液相色谱联用检测方法。聚(甲基丙烯酸-乙二醇二甲基丙烯酸酯)毛细管整体柱作为萃取介质,表现出较大的萃取容量。实验优化了影响萃取效率的参数,包括萃取流速、样品溶液pH值、盐浓度以及有机相含量。样品经过磷酸盐溶液稀释和过滤后便可直接进行萃取分析。睾酮、甲基睾酮和孕酮在10~1000μg/L的浓度范围内具有良好的线性关系,相关系数均大于0.996;它们的检出限分别为2.3,2.8和4.6μg/L;日内及日间相对标准偏差分别小于7.7%和7.5%。本方法已成功地应用到实际样品检测中,3种性激素的加标回收率为83%~119%。
A method was presented for the determination of testosterone, methyltestosterone and progesterone in liquid cosmetics by coupling polymer monolith microextraction (PMME) to high performance liquid chromatography with UV detection. A poly (methacrylic acid-ethylene glycol dimethacrylate ) monolithic capillary column was selected as the extraction medium, which showed high extraction capacity towards these compounds. To achieve optimum extraction performance, several parameters relating to PMME were investigated, including extraction flow rate and pH value, inorganic salt and organic phase concentration of the sample matrix. By simple dilution with phosphate solution and filtering, the sample solution then could be directly injected into the device for extraction. The limits of detection of testosterone, methyltestosterone and progesterone were calculated to be 2.3, 2.8 and 4.6 μg/L. Good linearity was achieved in the range of 10 to 1000 μg/L with a linear coefficient r value above 0.996. Excellent method reproducibility was found by intra- and inter-day precisions, yielding the relative standard ery for them in the real samples was between 83% deviations of 〈7.7% and 〈7.5%, respectively. Recovely for them in the real samples was between 83% and 119%.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2007年第5期681-684,共4页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金(No.20475040)
中国科学院知识创新工程重要方向项目(No.KSCX2-SW-128)
教育部"新世纪优秀人才支持计划"基金(No.NCET-05-0616)资助项目
关键词
聚合物整体柱微萃取
高效液相色谱
性激素
水性化妆品
Polymer monolith microextraction, high performance liquid chromatography, sexual hormones,liquid cosmetics
作者简介
E—mail:yqfeng@public.wh.hb.cn