昆明山海棠搽剂的研制和质量控制  

RPHPLC assay for determination of fluconazole in human serum and its pharmacokinetics and bioavailability investigations

作　　者：马文玺[1,2] 颉江敏[1,2] 

机构地区：[1]遵义医学院第一附属医院药剂科 [2]遵义医学院化学教研室

出　　处：《中国药学杂志》1998年第8期476-478,共3页Chinese Pharmaceutical Journal

摘　　要：目的：制备昆明山海棠搽剂用于治疗类风湿性关节炎，并建立检测方法，以控制其质量。方法：选用适当溶剂提取有效成分（生物碱和总萜内酯），按制剂学原理制成搽剂；薄层层析法定性检测；分光光度法测定含量。结果：薄层色谱中斑点清晰，易于识别；生物碱显色后在５００ｎｍ处测定吸光度Ａ１，Ａ１与其含量有良好的线性关系，线性范围０．１ｍｇ·ｍｌ－１～０．５ｍｇ·ｍｌ－１，平均回收率９６％～９８％，ＲＳＤ小于１．０％（ｎ＝３）；总萜内酯显色后在５３０ｎｍ处测定吸光度Ａ２，Ａ２与其含量线性相关，线性范围０．１μｇ·ｍｌ－１～０．５μｇ·ｍｌ－１，平均回收率１０４％～１０８％，ＲＳＤ小于１．９％（ｎ＝３）。结论：检测方法简单快捷，检测结果准确，重现性好。OBJECTIVE: To develope a sensitive RPHPLC method for the determination of fluconazole (FCZ) in human serum and to study its pharmacokinetics and bioavailability in human. METHOD: The drug was alkalized and extracted with ethyl acetate from serum and separated from endogenous interference on a Spherisorb C18 (200 mm×4.0 mm, 5μm) column with acetonitrilewaterphosphoric acid (250∶750∶1.2, pH was adjusted to 4 by diethyl amine). UV detector was set at 260 nm and triamterene was used as the internal standard. The data obtained were analyzed with Z89NLF program. RESULTS: A linear relationship was obtained between the peak area ratio and the concentration of FCZ from 0.25 to 10.0 μg·ml-1 and the lowest limit of detection of FCZ in serum was 0.1 μg·ml-1. Withinrun and betweenrun precisions were 6.30% (n=5) and 8.98% (n=5), respectively. The recoveries were 99.33%～102.28%. The one compartment open model with zero order absorption was used to described the time course of serum concentrations of FCZ in eight human volunteers following administration of a single oral dose (150 mg) as tablets. The results were tmax=1.69 h, cmax=3.30 μg·ml-1, t1/2=27 h and Frel=108.32%. CONCLUSION: The method is simple and accurate and is very suitable for the study of FCZ pharmacokinetics. The tested tablets and the reference capsules is bioequivalent.

关 键 词：昆明山海棠 搽剂 质量控制 TLC 分光光度法 

分 类 号：R286.0[医药卫生—中药学] R283.626[医药卫生—中医学]