高效液相色谱法测定人血浆中柳氮磺胺吡啶及其代谢物

Determination of sulfasalazine and its metabolite in plasma by HPLC

目的 :高效液相色谱法 (HPLC)测定人血浆中柳氮磺胺吡啶 (sulfasalazine,SASP)及其代谢物磺胺吡啶 (sulfapyridine,SP)的浓度。方法 :采用C1 8色谱柱 (4.6mm× 2 5 0mm ,5 μm) ,柱温 37℃ ,流动相为甲醇 - [乙酸铵 3.8g+四丁基溴化铵7.4 g、EDTA 0 .9g溶于 4 0 0mL的水中 ]5 5∶4 5 ,苯巴比妥作内标 ,检测波长 2 5 4nm。结果 :SASP和SP的线性范围分别为 1 .0～ 90 .0mg·L-1 ,1 .0～ 6 0 .0mg·L-1 ;平均回收率分别为 (1 0 2 .1± 4 .0 ) %,(1 0 1 .6± 4 .1 ) %;日内RSD <6 %,日间RSD <1 0 %。结论 :用HPLC法测定人血浆中SASP及其代谢物SP的浓度 ,结果可靠。

OBJECTIVE To determine sulfasalazine(SASP) and its metabolite sulfapyridine(SP) in plasma by HPLC. METHODS The method was paired ion chromatography, using phenobarbital as internal standard. The conditions included ODS column( 4.6 mm × 250 mm , 5 μm ) , the mobile phase consisted of methanol:[ammonium acetate 3.8 g , tetrabutylammonium bromide 7.4 g ,EDTA 0.9 g in water 400mL] (55∶45), UV detector was set at 254 nm and the injection volume was 20μL .RESULTS Under this condition, the linear concentration range was 1.0 ～ 90.0 mg ·L -1 for SASP and 1.0 ～ 60.0 mg ·L -1 for SP, the averages of recovery was ( 102.1 ± 4.0)% for SASP and ( 101.6 ± 4.1)% for SP, respectively, and RSDs were less then 10%. CONCLUSIONS The proposed method is selective, simple and accurate. The result was satisfactory.