高灵敏度微量高效液相色谱法分析中样品吸附和进样残留  

The adsorption and injector's carry over' in highly sensitive HPLC determination

作　　者：施孝金[1] 陈妙英[1] 张静华[1] 王宏图[1] 

机构地区：[1]上海医科大学华山医院临床药学研究室,上海200040

出　　处：《中国临床药学杂志》1999年第S1期33-36,共4页Chinese Journal of Clinical Pharmacy

摘　　要：目的:解决高灵敏度微量HPLC分析中样品吸附和进样残留问题.方法:用荧光检测、全自动进样的HPLC分析法对胰岛增敏剂(RGL)分析过程使用的容器、自动进样器使用的清洗液种类、自动清洗程序进行考察.结果:当RGL浓度<10ng/ml时,玻璃试管对RGL的吸附率达9.54%,而用聚丙烯试管的吸附率为0.53%.当进样上柱量500ng时,用清洗液甲醇/水(90/10)经自动标准清洗程序清洗1次后,RGL残留0.27ng(以相对峰面积计算);改进清洗程序加用流动相清洗六通阀,清洗1次后,RGL残留小于0.055ng.结论:聚丙烯容器可避免RGL的吸附损失,改进自动清洗程序可解决进样残留对分析的影响.AIM:To study the adsorption and auto-injector's 1 'carry over' in highly sensi-tive HPLC assay. METHODS: By using HPLC with auto-injector and fluorescence detector for the determination of rosiglitazone(RGL), we observed adsorption actions of the tubes and auto-injector,and eluting effects of washing solvent and washing program parameters. RE-SULTS: When the RGL concentration was less than 10 ng/ml,its adsorption rates of glass and polypropylene tubes were 9. 54 % and 0. 53% , respectively. By using modified washing program parameters instead of the default parameters, the residues of RGL were changed from 0. 27 ng to 0. 055 ng in auto-injector because of 'carry over' when the quantity injected in the column was more than 500ng. The eluting effect of methanol/water(90/l0,V/V) wasthe best if comparing with acetonitrile, methanol, hexane, trichloromthane and the mobil phase. CONCLUSION: Polypropylene tubes is the best for RGL assay with a minimal ad-sorption rate. The auto-injector's 'carry over' are clear out by improving the washing program parameters and washing solvent.

关 键 词：吸附 高效液相色谱 胰岛增敏剂 

分 类 号：O657.7[理学—分析化学]