摘要
以5-溴尿嘧啶为内标,建立了高效液相色谱法测定小鼠组织中肝靶向前药(半乳糖化人血清白蛋白与5-氟尿嘧啶偶联物)中5-氟尿嘧啶(5-Fu)含量的分析方法。样品经盐酸水解、乙酸乙酯提取、离心后,取上清液在40℃下用N2吹干,用流动相溶解、定容后进样分析。色谱条件:安捷伦Hypersil C18色谱柱(4.0mm×250mm,5μm),流动相为甲醇-磷酸缓冲溶液,流速0.7mL/min,UV检测波长为270nm。方法的线性范围为1~20mg/L,检出限(S/N=3)为0.1mg/L,回收率为93%~104%。该法操作简便、灵敏度高,适于组织中肝靶向前药半乳糖化人血清白蛋白与5-氟尿嘧啶偶联物(Gal—HSA-5-FU)的5-Fu含量测定。
5-Fluorouracil A high performance liquid chromatography method was developed for the determination of 5-fluorouraeil (5-FU) in galactosylated human serum albumin 5-fluorouracil conjugate ( Gal-HSA - 5-FU), one kind of the hepatic target predrug, in mice tissues by using 5-bromine uracil(5-BrU) as internal standard. The sample was hydrolyzed by hydrochloric acid, extracted by ethyl acetate and separated by centrifugation. The supernatant was dried by nitrogen gas at 40 ℃, dissolved by methanol- phosphoric acid buffer. The chromatographic analysis was performed on an Agilent Hypersil C18 column(4.0 mm× 250 mm, 5 μm) with methanol -phosphoric acid buffer solution as mobile phase. The flow rate for mobile phase was 0. 7 mL/min and the detection wavelength was set at 270 nm. The linear range was 1 -20 mg/L with the detection limits of 0. 1 mg/L( S/N = 3 ), and the recoveries for the method were between 93% - 104% . The method was simple, sensitive and applicable to determine the 5-FU content of hepatic target predrug in tissues.
出处
《分析测试学报》
CAS
CSCD
北大核心
2009年第6期746-748,共3页
Journal of Instrumental Analysis