在线SPE-HPLC技术检测血浆中NK-1浓度的研究  

Study on the detection of plasma NK-1 concenlration online in SPE-HPLC Technology

作　　者：杨小宁 郭伟康[2] 韩梅梅[3] 张瀚文[2] 王国敏[2] 卢亚欣[2] 

机构地区：[1]天津和美生物技术有限公司,天津300192 [2]南开大学药学院,天津300071 [3]通化市第二人民医院药剂科,通化134003

出　　处：《北方药学》2014年第9期79-81,共3页Journal of North Pharmacy

摘　　要：目的：建立NK-1的在线SPE-HPLC血浆样品检测方法。方法：采用在线SPE-HPLC技术测定小鼠血浆中NK-1浓度。预处理柱：CAPCELL PAK MF Ph-1色谱柱（4.6mm×10mm）,色谱分析柱：Venusil MP C18（5μm,100,4.6mm×150mm）,预处理流动相：20mM磷酸盐缓冲液（pH值=2.8）,分析流动相：20mM磷酸盐缓冲液（pH值=2.8）∶乙腈（70∶30,v/v）,检测波长：270nm,柱温：30℃。结果：本方法线性范围25～1000ng·ml-1,最低检测限2ng·ml-1,r=0.9994；日内、日间精密度分别小于5.0%和6.0%；高、中、低3个浓度的QC样品：方法回收率分别为103.25±2.98%、97.21±4.06%、102.35±2.64%。结论：本法测定血浆中NK-1含量准确、简便,适用于NK-1药物动力学的研究。Objective： To establish a On-Line SPE-HPLC method for the determination of NK-1 in mouse plasma. Methods： The Automated On-Line SPE-HPLC system loads the plasma samples automatically, while a CAPCELL PAK MF Ph-1 pre-column（4.6mm×10mm）excludes the macromolecules and focuses the analyses by a mobile phase consisting in phosphate buffer （20mM, pH/值=2.8）; afterwards, a second mobile phase consisting in a mixture of phosphate buffer（20mM, pH 值=2.8）and acetonitrile（70：30, v/v）elutes the analyses to a Venusil MP Ci8 （5μm, 100k, 4.6mm×150mm）analytical column in back flush mode at flow rate of 1 ml＇min-I. The UV detection was performed at 270 nm. The column temperature was 30℃. Results： The calibration calve was linear within the range of 25- 1000ng·ml-1, the detection limit was 2ng·ml-1 （S/N=3）,r=0.9994; the inter-day and intra-day RSD% was less than 5.0% and 6.0% , respectively; for QC samples at 1000ng·ml-1, 200ng·ml-1 and 25ng·ml-1, the method recovery was 103.25±2.98%, 97.21_＋4.06%, 102.35＋2.64%, respectively. Conclusion： The method is simple with high sensitivity and good precision and has proved to be suitable for pharmacokinetic study of ADOX in mouse plasma.

关 键 词：NK-1 在线 SPE-HPLC技术 药物动力学 系统峰 

分 类 号：R969.1[医药卫生—药理学]