HPLC-MS/MS 测定大鼠肝脏组织中丹参素钠的浓度

王晶; 董昕; 邹豪; 金磊; 张川

HPLC-MS/MS 测定大鼠肝脏组织中丹参素钠的浓度

投稿时间：2011-04-21 修订日期：2011-06-14 点此下载全文

引用本文：王晶,董昕,邹豪,金磊,张川.HPLC-MS/MS 测定大鼠肝脏组织中丹参素钠的浓度[J].药学实践杂志,2012,30(1):52~54

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作者	单位	E-mail
王晶	第二军医大学药学院新药研究中心,上海 200433 上海市中山医院青浦分院药剂科,上海 201700
董昕	第二军医大学药学院分析测试中心,上海 200433
邹豪	第二军医大学药学院新药研究中心,上海 200433
金磊	第二军医大学药学院新药研究中心,上海 200433
张川	第二军医大学药学院新药研究中心,上海 200433	zhangchuan@smmu.edu.cn

基金项目:上海市中药现代化专项基金(08DZ1970802).

中文摘要:目的建立液质联用色谱法(HPLC-MS/MS)测定SD大鼠肝脏组织中丹参素钠的浓度。方法肝脏组织样品制成匀浆后,加入内标酮洛芬,采用液液萃取方法进行预处理。色谱柱:Diamonsil C₁₈柱(200 mm×4.6 mm ,5 μm);流动相:甲醇-水(含0.01‰甲酸)(80:20);流速:1.0 ml/min;质谱条件:采用ESI离子源,负离子检测,选择MRM 测定丹参素钠和酮洛芬197→135 m/z 和 253→209 m/z。结果丹参素钠在20.2~1 010 n

中文关键词:液质联用色谱法丹参素钠组织浓度

Determination of sodium Danshensu in rat liver by HPLC-MS/MS

Abstract:Objective To establish a HPLC-MS/MS method for determination of sodium Danshensu in SD rat liver. Methods Tissue samples were pretreated by liquid-liquid extraction method after homogenate, and ketoprofen was used as the internal standard. Analytical column was Diamonsil C₁₈ (200 mm×4.6 mm, 5 μm). The mobile phase was methanol: water(0.01‰ formic acid)=80:20 with flow rate as 1.0 ml/min. Mass spectrum determination was performed in the MRM mode with target ions m/z 197→135 (Sodium Danshensu), m/z 253→209 (ketoprofen), using ESI ion resource and negative ion detection. Results The calibration curve was linear over the range of 20.2~1 010 ng/ml. The LLOQ of sodium Danshensu in liver was 20.2 ng/ml. The intra-and inter-day RSD were both less than 10%. The extracted recovery rate ranged from 92% to 107%. Conclusion The method was sensitive, rapid, simple and accurate to determine sodium Danshensu distribution in rat liver and was suitable for preclinical test of Sodium Danshensu.

keywords:HPLC-MS/MS sodium Danshensu drug concentration in tissue

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