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首页> 外文期刊>Journal of liquid chromatography and related technologies >Determination of Methimazole in Pharmaceutical Preparations using an HPLC Method Coupled with an Iodine-Azide Post-Column Reaction
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Determination of Methimazole in Pharmaceutical Preparations using an HPLC Method Coupled with an Iodine-Azide Post-Column Reaction

机译:HPLC法与叠氮化碘后柱反应联用测定药物制剂中的甲咪唑

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A simple and reliable high performance liquid chromatographic (HPLC) method with iodine-azide post-column reaction as a detection system has been developed and validated for determination of methimazole in tablets. A chromatographic separation was achieved on a Cig column with a mobile phase consisting of acetonitrile, water, and 2.5% sodium azide solution (pH 5.5) with isocratic elution (20:30:50, v/v/v). The detection is based on spectrophotometric measurement of the residual iodine (2 = 350nm) from the post-column iodine-azide reaction induced by methimazole, after mixing an iodine solution containing iodide ions with the column effluent containing azide ions and methimazole. Obtained chromatograms for methimazole showed negative peaks as a result of the decrease in background absorbance. The method developed for methimazole was linear over the concentration range of 0.2-2 祄ol L. The method is accurate and precise (relative standard deviation, R.S.D. < 4%). The detection limit (defined as S/N = 3) was 0.18 祄ol L-1 (3.6pmol injected amount) for the described compound. The elaborated method was applied to determine methimazole in tablets.
机译:开发了一种简单可靠的高效液相色谱(HPLC)方法,其中碘叠氮化物柱后反应作为检测系统,并已用于测定片剂中甲巯咪唑的有效性。在Cig柱上进行色谱分离,流动相由乙腈,水和2.5%叠氮化钠溶液(pH 5.5)组成,等度洗脱(20:30:50,v / v / v)。该检测基于分光光度法测量,该分光光度法是在将含有碘离子的碘溶液与含有叠氮离子和甲met唑的柱流出物混合后,从由甲him唑引起的柱后碘叠氮化物反应中残留碘(2 = 350nm)进行测量。由于背景吸光度降低,获得的甲巯咪唑色谱图显示负峰。甲硫咪唑开发的方法在0.2-2 olol L的浓度范围内是线性的。该方法准确,准确(相对标准偏差,R.S.D。<4%)。该化合物的检出限(定义为S / N = 3)为0.18 mol L-1(3.6pmol注入量)。采用改进的方法测定片剂中的甲巯咪唑。

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