高效液相色谱法测定抗癌原料药芳香异羟肟酸二丁基锡  

Determination of organometallic antitumor crude drug arylhydroxamic acid of dibutyltin(Ⅳ) by high-performance liquid chromatography

作　　者：李云兰[1] 王晓剑[1] 杨莉[1] 李青山[1] 

机构地区：[1]山西医科大学药学院,太原030001

出　　处：《分析试验室》2007年第8期21-24,共4页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金青年基金(39900185);国家教育部新世纪优秀人才支持计划(NCET-04-0258);山西医科大学大学生创新基金;太原市大学生创新创业扶持;山西高校科技研究开发项目资助

摘　　要：建立了反相高效液相色谱法测定有机金属抗癌原料药芳香异羟肟酸二丁基锡。色谱条件：Diamonsil ODS色谱柱（4.6 mmi.d.×200 mm，5μm），以V（甲醇）∶V（水）=35∶65，pH2.5为流动相，流速为1.0 mL/min，紫外检测波长232 nm，柱温25℃。吲达帕安为内标测定芳香异羟肟酸二丁基锡。结果表明：线性范围为4.08-102μg/mL，回归方程为f=0.02253ρ-0.005843，r=0.9998（n=7），方法精密度RSD为0.89%（n=6），稳定性的RSD为0.56%（n=9），重复性的RSD为0.90%（n=9），平均回收率为100.5%（n=9，RSD=1.1%）。方法可用来测定芳香异羟肟酸二丁基锡。A method for the determination of a novel organometallic antitumor crude drug arylhydroxamic acid of dibutyltin（Ⅳ） by reversed-phase high-performance liquid chromatography was established. A Shimadzu LC-10ATvp HPLC system was adopted with Diamonsil ODS （4.6 mm ×200 mm, 5 μm） as the stationary phase. The mobile phase was consisted of methanol and water （35 ： 65, pH 2.5） at a flow rate of 1.0 mL/min. The UV detection wavelength was set at 232 nm and the column temperature was 25 ℃. Indapamide was selected as an internal standard to determine the concentration of arylhydroxamic acid of dibutyltin. Under the selected chromatographic conditions, there was the good separation efficiency between the internal and the sample. The linear range was 4.08 - 102 μg/mL, and regression equation was f= 0.02253c - 0.005843 （c： μg/mL）, r = 0.9998 （ n = 7）. The RSD of precision was 0.89% （ n = 6）. The RSDs of stability and reproducibility were 0.56% and 0.9% （ n = 9）, respectively. The average recovery was 100.5% （ n = 9, RSD = 1.1% ）. The analytical method is accurate, sensitive and selective for the analysis of the content of novel organometallic antitumor crude drug arylhydroxamic acid of dibutyltin（ Ⅳ ）.

关 键 词：芳香异羟肟酸二丁基锡 反相高效液相色谱法 含量测定 

分 类 号：O657.7[理学—分析化学]