基于溴甲酚绿和溴甲酚紫离子对反应的药物中磷酸氯喹的灵敏、选择性无萃取分光光度测定

Nagib Qarah As, K. Basavaiah, N. Swamy
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引用次数: 5

摘要

磷酸氯喹(Chloroquine Phosphate, CQP)是一种广泛用于治疗疟疾的抗疟药。采用溴甲酚绿(BCG法)和溴甲酚紫(BCP法)两种磺胺苯酞染料,建立了两种快速、简便、选择性和灵敏度高的测定原料药和剂型CQP的分光光度法。当CQP与任何一种染料反应时,两种方法都是基于氯仿可溶性离子对的形成,两种方法都适用于420 nm的测量。对反应时间、染料浓度、反应介质等因素的影响进行了研究和优化。在最佳反应条件下,BCG法和BCP法CQP(碱)的过浓度范围分别为1 ~ 20 μg和0.5 ~ 12 μg mL-1,符合Beer定律,相应的摩尔吸光度值分别为1.79 × 104和3.09 × 104 L mol-1 cm-1。计算检出限(LOD)和定量限(LOQ)分别为0.27和0.82 μ mL-1 (BCG法);0.15、0.46 μ mL-1 (BCP法)。日内和日间%RSD值分别≤1.56%和≤1.83%,%RE值均优于2%。方法的稳健性是通过在稍微改变的最佳条件下进行分析来确定的,而坚固性是通过人员之间以及设备之间的变化来测试的;在这两种情况下,%RSD值都在可接受的范围内。方法的选择性通过安慰剂空白和合成混合物分析确定,在试验中没有可检测到的共配制物质的干扰。将该方法应用于中药片剂、混悬液和注射剂的含量测定,结果满意。通过标准加入法进行回收率试验,证实了该方法的准确性。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Sensitive and Selective Extraction-Free Spectrophotometric Assay ofChloroquine Phosphate in Pharmaceuticals Based on Ion-Pair Reactionwith Bromocresol Green and Bromocresol Purple
Chloroquine Phosphate (CQP) is an antimalarial agent extensively used in the treatment of malaria. Two spectrophotometric methods, which are rapid, simple, selective and sensitive, are presented for the determination of CQP in bulk and dosage forms using two sulphonphthalein dyes: Bromocresol Green (BCG method) and Bromocresol Purple (BCP method). The methods are based on the formation of chloroform-soluble ion-pairs, when CQP is reacted with either dye, suitable for measurement at 420 nm in both the methods. The effects of reaction time, dye concentration and reaction medium were carefully studied and optimized. Under the optimum reaction conditions, Beer's law is obeyed overconcentration ranges 1-20 and 0.5-12 μg mL-1 CQP (base) for BCG method and BCP method respectively, with corresponding molar absorptivity values of 1.79 × 104 and 3.09 × 104 L mol-1 cm-1. The calculated limits of detection (LOD) and quantification (LOQ) are 0.27 and 0.82 μg mL-1 (BCG method); 0.15 and 0.46 μg mL-1 (BCP method). Intra-day and inter-day %RSD values were ≤1.56% and ≤1.83% whereas the respective %RE values were better than 2%. Robustness of the methods was determined by performing analysis with slightly altered optimum conditions while ruggedness was tested by inter-personnel as well as inter-equipment variations; the %RSD values were within the accepted limits in both instances. Method selectivity was as ascertained by placebo blank and synthetic mixture analysis with no detectable interference from co-formulated substances in the assays. The methods were applied to the determination of CQP in tablets, suspension and injections with satisfactory results. Accuracy was also confirmed by recovery test via standard-addition procedure.
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