摘要
基于异烟肼和利福平在碱性介质中能与K3Fe(CN) 6 反应产生强的化学发光 ,因此设计了一个经高效液相色谱(HPLC)分离柱后同时检测一线抗结核病药物异烟肼、利福平的化学发光检测器 .研究并优化了流动相、流速以及化学发光检测的条件 .该方法测定异烟肼、利福平的线性范围分别为 0 .0 5～ 6.0mg L ,0 .0 8～ 2 0 .0mg L ,其检出限 :异烟肼为 2× 10 - 2mg L ,利福平为 4× 10 - 2 mg L ,测定的相对标准偏差分别为 1.9% ,2 .9% .
A novel chemiluminescence reaction detector was developed for the simultaneous determination of isoniazid (INH) and rifampin (UP), which are the two most active first-line drugs for treatment of tuberculosis, separated by HPLC based on the direct hexacyanoferrate (III) chemiluminescence reaction by isoniazid and rifampin in sodium hydruaide medium. The separation was carried out on Kromasil RP-C-18 column (150 mm X 4. 6 mm i. d., 5 mum) at 35 degreesC. The mobile phase consisted of a V(methanol) : V(water) = 60: 46 solution. At a flow-rate of 0.8 mL/min. the total run time was similar to 6 min. Parameters affecting CL detection, such as CL reaction reagent [K3Fe(CN)(6)] concentration, sodium hydroxide and methanol concentration were optimized. The chemiluminescence intensity was linear with isoniazid and rifampin concentration in the range of 0.05 similar to 6.0 mg/L and 0.08 similar to 20.0 mg/L, respectively. The limits of detection (LOD) for isoniazid and rifampin were 2 x 10(-2) mg/L and 4 x 10(-2) Mg/L, respectively. The relative standard deviation ( n = 11) was 1.9% for 0.1 mg/L isoniazid and 2.9% for 1.0 mg/L rifampin, respectively. The recovery was in the range of 97.8% similar to 105.2%. The proposed method has been applied satisfactorily to the determination of isoniazid and rifampin in the compoud tablets of rifampin.
出处
《化学学报》
SCIE
CAS
CSCD
北大核心
2003年第2期303-306,共4页
Acta Chimica Sinica
基金
国家自然科学基金 (No.2 0 1 750 39)资助项目
