Standardization of Some Commercial Anti-diabetic Herbal Products containing Syzygiumcumini

An isocratic HPLC method was developed for standardization of five commercially available products containing S. cumini seeds (DIABECON, MADHULENE, HYPONIDD, D-FIT and DIABEGON)using methylxanthoxylin (MXX)as marker. The method was validated in accordance with ICH Q2(R1) guidelines. The chromatographic separation of MXX was achieved on a C18 column by mobile phase composed of methanol and water (60:40%v/v) at a flow rate 0.5 mL/min. The eluent was detected at 280 nm.The method was linear over concentration of 1-200 μg/mL with correlation coefficient of 0.9999. The LOD and LOQ were 0.175 and 0.530 µg/mL, respectively. The method was precise (%RSD <0.31), accurate and robust for determination of MXX in herbal extracts. The content of MXX in the seed extract was found to be 0.0433%w/w while it was ranging from 0.026-0.041%w/w in the products. The content of MXX was found to be equivalent to the pure seed extract only in DIABECON tablets and D-FIT soft gelatine capsules while it was found to be significantly less in the other formulations

Degradation Study on Sulfasalazine and a Validated HPLC-UV Method for its Stability Testing

Sulfasalazine (SSZ) was subjected to degradation under the conditions of hydrolysis (acid, alkali, and water), oxidation (30% H2O2), dry heat, and photo-lysis (UV-VIS light) in accordance with the ICH guidelines. An RP-HPLC method was developed to study the degradation behavior. No degradation was noted under any condition except alkaline hydrolysis where SSZ was degraded to a single minor product. SSZ was optimally resolved from this product on an XTerra® RP18 column with a mobile phase composed of methanol and an ammonium acetate buffer (10 mM, pH 7.0) (48:52, v/v) delivered at a rate of 0.8 mL/min in an isocratic mode. The method was validated and found to be linear (r2=0.99945), precise (%RSD <2), robust, and accurate (94–102%) in the concentration range of 0.5–50 μg/mL of SSZ. The PDA analysis of the degraded sample revealed the SSZ peak purity to be 998.99 and the drug peak eluted with a resolution factor of >2 from the nearest resolving peak, indicating the method to be selectively stability-indicating for the drug analysis. The method was applied successfully for the stability testing of the commercially available SSZ tablets that were under varied ICH-prescribed conditions. An explanation for the unusual stability of the drug when exposed to acidic hydrolysis, despite the presence of the sulfonamide linkage, is also discussed

Isolation and characterization of a degradation product in leflunomide and a validated selective stability-indicating HPLCâUV method for their quantification

Leflunomide (LLM) is subjected to forced degradation under conditions of hydrolysis, oxidation, dry heat, and photolysis as recommended by International Conference on Harmonization guideline Q1A(R2). In total, four degradation products (IâIV) were formed under different conditions. Products I, II and IV were formed in alkaline hydrolytic, acidic hydrolytic and alkaline photolytic conditions. LLM and all degradation products were optimally resolved by gradient elution over a C18 column. The major degradation product (IV) formed in hydrolytic alkaline conditions was isolated through column chromatography. Based on its 1H NMR, IR and mass spectral data, it was characterized as a British Pharmacopoeial impurity B. The HPLC method was found to be linear, accurate, precise, sensitive, specific, rugged and robust for quantification of LLM as well as product IV. Finally, the method was applied to stability testing of the commercially available LLM tablets. Keywords: Leflunomide, Characterization, Forced degradation, Degradation product, HPLCâU

Identification and characterization of degradation products of Nateglinide

Nateglinide (NTG) was evaluated under a variety of ICH-recommended forced degradation settings and found to be degraded under acid and alkali hydrolysis but stable under other forced degradation conditions. Under acid hydrolytic conditions, three degradation impurities (I-III) were produced. All three contaminants were separated using a C-18 column with ammonium acetate buffer (20 mM), methanol, and acetonitrile as mobile phases provided in isocratic mode, and characterisation was done utilising +ESI-MSn and LC-MS-QTOF investigations. All three degrading impurities (I-III) were discovered to be novel. The most likely pathways of deterioration were presented and debated.&nbsp

Identification and Characterization of Degradation Products of Nateglinide

Nateglinide (NTG) was evaluated under a variety of ICH-recommended forced degradation settings and found to be degraded under acid and alkali hydrolysis but stable under other forced degradation conditions. Under acid hydrolytic conditions, three degradation impurities (I-III) were produced. All three contaminants were separated using a C-18 column with ammonium acetate buffer (20 mM), methanol, and acetonitrile as mobile phases provided in isocratic mode, and characterisation was done utilising +ESI-MSn and LC-MS-QTOF investigations. All three degrading impurities (I-III) were discovered to be novel. The most likely pathways of deterioration were presented and debated.&nbsp