A NEW RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS ESTIMATION OF KETOROLAC TROMETHAMINE AND TRAMADOL HYDROCHLORIDE IN PHARMACEUTICAL DOSAGE FORMS.

Objective: This study was embarked upon to develop a new, simple, rapid, validated reversed-phase high-performance liquid chromatography (HPLC)method for the estimation of ketorolac tromethamine (KET) and tramadol hydrochloride (TDL) in pharmaceutical dosage forms.Methods: The HPLC method was developed on Shishiedo C18 column (250 mm × 4.6 mm i.d, 5 μ) using methanol: 50 mM phosphate buffer (pH 6.0) in the ratio of 52:48 at 282 nm.Results: Retention time for the drugs was found to be 5.1 and 6.9 minutes for tramadol and ketorolac, respectively. The limit of detection for tramadoland ketorolac were found to be 1.0 and 0.1 μg/ml, limit of quantitation for tramadol and ketorolac were found to be 5.0 and 0.5 μg/ml, respectively. Linearity was established in the range of 20.0-30.0 μg/ml and 8.0-12.0 μg/ml for TDL and KET, respectively. The method was precise with % relative standard deviation <2 for both intra- and interday precision. The accuracy of the method was performed over three levels of concentration, and the recovery was in the range of 98-102%.Conclusion: From the found experimental data, it can be concluded that the developed method is accurate, precise, and selective and can be employedsuccessfully for the estimation of KET and TDL in Pharmaceutical dosage forms.Â

An expeditious synthesis of imides from phthalic, maleic and succinic anhydrides and chemoselective C=C reduction of maleic amide esters

392-398Phthalic, maleic and succinic anhydrides have been reacted with<span style="mso-fareast-font-family:Calibri;mso-ansi-language: EN-IN"> aromatic amines to obtain the corresponding monoacid monoamides.<span style="mso-fareast-font-family: Calibri;mso-ansi-language:EN-IN" lang="EN-GB"> The latter have been each transformed into the corresponding cyclic imide derivatives by treating with SOCl2. Alternatively,<b style="mso-bidi-font-weight: normal"> anhydrides have been<span style="mso-fareast-font-family:Calibri;mso-ansi-language: EN-IN"> reacted with methanolic KOH to obtain monomethyl ester derivatives which on reaction with aromatic amines in the presence of EDC. HCl and HOBt <span style="mso-fareast-font-family:Calibri; mso-ansi-language:EN-IN">give cyclic imide derivatives. Reaction of monoacid monoamides<span style="mso-fareast-font-family:Calibri; mso-ansi-language:EN-IN"> independently, with SOCl2 at 0-5°<span style="mso-fareast-font-family:Calibri;mso-ansi-language: EN-IN">C give the monoamide monoester derivatives.<span style="mso-fareast-font-family:Calibri;mso-ansi-language:EN-IN;mso-fareast-language: EN-IN"> Treatment of <span style="mso-fareast-font-family: Calibri;mso-ansi-language:EN-IN">monoamide monoester of malic anhydride with NaBH4 leads to the unusual reduction of C=C grouping as well as the carbonyl group of the ester group to from monoamide monoalcohol of succinic anhydride. Preparation of monoamide monoalcohol of succinic anhydride can also be achieved by chemoselective reduction of <span style="mso-fareast-font-family: Calibri;mso-ansi-language:EN-IN">monoamide monoester of malic anhydride with Mg turnings yielding <span style="mso-fareast-font-family: Calibri;mso-ansi-language:EN-IN">monoamide monoester of succinic anhydride followed by reduction of the latter with NaBH4. </span