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A first order derivative UV-spectrophotometric method for the determination of diltiazem hydrochloride and mexiletine hydrochloride has been developed and validated. In the assay, the first- and second-order measurements with the use of the "peak-zero" and "peak-peak" techniques were applied. The linear correlation (r < 0.9999) between the amplitude of the peak and the concentration of the examined drugs in the range of 3.0-8.0 microg mL(-1) for diltiazem and 50-100 microg mL(-1) for mexiletine was obtained. The proposed method was successfully applied for accurate (mean recovery about 100%), precise (RSD about 1%) and selective determination of the studied drug in the pure and dosage forms.

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