HPLC-FLD法测定犬血中盐酸哌唑嗪的浓度  

HPLC-FLD Determination of Prazosin Hydrochloride in Plasma of Dog

作　　者：许茜[1] 余书勤[2] 潘莹宇[1] 陆晶[2] 

机构地区：[1]东南大学公共卫生学院,南京210009 [2]南京师范大学生命科学院,南京210097

出　　处：《药物分析杂志》2005年第11期1325-1328,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立测定犬血中盐酸哌唑嗪浓度的高效液相色谱法,以进行哌唑嗪制剂的犬生物利用度研究。方法:取犬血浆0.5mL,加2mol·L^(-1)氢氧化钠溶液100μL,加内标100μL(20.0μg·mL^(-1)奎宁溶液),混匀,然后加入乙醚3 mL,涡旋振荡、离心,分出有机相,40℃水浴氮气流吹干,用流动相100μL溶解残渣,取上清液20μL进行 HPLC 分析。流动相为 pH 3.6醋酸-醋酸钠缓冲液-乙腈(70:30),流速为1.0 mL·min^(-1),色谱柱为迪马公司 Diamond C_(18)柱(250mm×4.6mm,4.0μm),柱温20℃。荧光激发波长为258nm,荧光发射波长为387nm。结果:犬血浆中杂质不干扰样品的测定,犬血浆中哌唑嗪浓度在1.0～1000.0 ng·mL^(-1)范围内线性关系好(r=0.9998);最低检测浓度为1.0 ng·mL^(-1);方法的平均相对回收率大于90%;平均提取回收率高于80%;日内和日间 RSD 均小于10%。结论:所建立方法准确可靠,符合生物样品分析要求。Objective：To establish an method for the determination of harmacokinetics of p razosin hydrochloride. Methods：Mter the addition prazosin in plasma of dog, and studying p of quinine （ internal standard）, plasma （0. 5 mL） samples were extracted into aether. The residue after evaporation of the organic layer was dissolved in 100μL of mobile phase and 20 μL was injected on to HPLC. The separation was achieved using a Diamond C18 column（250 mm ×4. 6 mm,4. 0 μm）with a mobile phase composition of acetate buffer（ pH 3.6 ） -acetonitrile （70：30 ）. The flow - rate of the mobile phase was set at 1.0 mL · min^ - 1. The column eluate was monitored by fluorescence detector set at an excitation wavelength of 258 nm and emission wavelength of 387 nm. Results： Linear relationships （ r = 0. 9998）were observed between the peak area ratio prazosin to internal standard vs prazsion concentrations across the concentration range of 1.0 - 1000. 0 ng · mL^ - 1. The inter - day and intra - day precision was less than 10%. The extraction efficiency was more than 80% for both prazosin and internal standard from plasma. The lower limit of quantitation of the assay was 1.0 ng · mL^-1. Conclusions：The methodology for prazosin measurement in plasma is simple, sensitive and accurate.

关 键 词：哌唑嗪 HPLC—FLD 浓度测定 犬血浆 

分 类 号：R988.1[医药卫生—药品] R123.5[医药卫生—药学]