具選擇性且穩定之鹽酸可樂定檢測方法   全文下載

Selective Stability-Indicating Methods for the Determination of Clonidine Hydrochloride and/or Its Related Substance, 2,6-Dichloroaniline

本研究開發三種快速、靈敏度高且具選擇性之方法，檢測鹽酸可樂定及其相關物質2,6-二氯苯胺，第一種方法依據衍生物比率分光光度學，於首次衍生訊號，比率光譜波長228.4 nm（Δλ = 2 nm）時，測定鹽酸可樂定。 第二種方法於波長300.8 nm時檢測2,6-二氯苯胺的首次衍生反應，並不受鹽酸可樂定干擾。第三種方法，2,6-二氯苯胺經由重氮化並與n-(1-naphthyl) ethylenediamine作用，於波長498 nm時產生偶氮染料。每個方法的不同參數都經探討並最優化，且依據美國藥典準則，就線性、範圍、準確度，精密度，偵測和定量極限等方面確效。以衍生物比率分光光度法分析鹽酸可樂定錠劑，其結果與美國藥典第30版HPlC方法檢驗結果相符。第二及第三種方法可自鹽酸可樂定原料藥中檢測出2,6-二氯苯胺。"

Three rapid, sensitive and selective analytical methods were developed for the determination of clonidine hydrochloride and its related substance: 2,6-dichloroaniline in a mixture of both. The first method depends on derivative-ratio spectrophotometry where the first derivative signals of the ratio spectra at 228.4 nm (Δλ = 2 nm) were selected to determine clonidine hydrochloride. The second method is based on measuring the first derivative response of 2,6-dichloroaniline at 300.8 nm with no interference from intact clonidine hydrochloride. In the third method, 2,6-dichloroaniline was determined via diazotization and coupling with N-(1-naphthyl) ethylenediamine to yield a colored azo dye which was measured at 498 nm. Various parameters affecting each method were studied and optimized. The proposed methods were validated according to USP guidelines concerning linearity, ranges, accu-racy, precision, detection and quantification limits. The derivative-ratio spectrophotometric method was applied to the analysis of clonidine hydrochloride in tablets and the results were found in good agreement with those of the USP XXX HPLC procedure, while both the second and third methods permitted the selective analysis of 2,6-dichloroaniline in clonidine hydrochloride raw material.