将发光试剂钌(Ⅱ)联吡啶固定在离子交换树脂上,在酸性高锰酸钾氧化条件下,用于测定人血清中的雷尼替丁(RAN)。使用BDS C18柱为固定相,流动相为甲醇-磷酸盐缓冲溶液(pH 3.0)(35:65,V/V)。雷尼替丁的质量浓度在2.0×10-4~4.0×10-2mg/mL范围内呈良好的线性,回归方程为ΔICL=15.016ρ+187.09(r=0.9981)。检出限(3σ)为67 ng/mL。对2.0μg/mL的雷尼替丁进行11次平行测定,其相对标准偏差为2.2%。
A novel method was developed for the determination of ranitidine by high performance liquid chromatography(HPLC) with chemiluminescence(CL) detection.The chromatographic separation was performed on a Hypersil BDS-C18 column(i.d.: 250 mm×4.6 mm,particle size: 5 μm,pore size: 100) with an isocratic mobile phase consisting of methanol and 0.02 mol/L KH2PO4(pH 3.0)(volume ratio 35:65) at a flow rate of 1.0 mL/min.The detection was based on the chemiluminescence reaction of ranitidine with acidic potassium permanganate(KMnO4) and tris(2,2(-bipyridyl)ruthenium(III),which was immobilized on the cationic ion-exchange resin.Under optimum conditions,the linear range for ranitidine was 2.0×10-4~4.0×10-2 mg/mL with the detection limit of 67 ng/mL(3σ).The relative standard deviation(RSD) was 2.2%(n=11) for 2.0 μg/mL ranitidine.Ranitidine in the serum samples was analyzed by the proposed method with satisfactory results.