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Identification and Structure Elucidation of Forced Degradation Products of the Novel Propionic acid Derivative Loxoprofen: Development of Stability-Indicating Chromatographic Methods Validated as per ICH Guidelines.
J Chromatogr Sci 2017; 55(4):417-428JC

Abstract

Loxoprofen sodium (LOX) is a recently developed novel propionic acid derivative. Owing to its instability under both hydrolytic and oxidative conditions, the development of simple, rapid and sensitive methods for its determination in the presence of its possible forced degradation products becomes essential. Two simple chromatographic methods, high-performance thin layer chromatography (HPTLC) and high-performance liquid chromatography (HPLC), were developed associated with ultraviolet (UV) detection. In HPTLC-densitometric method, the separation of LOX from its degradation products was achieved using silica gel F254 plates and toluene:acetone:acetic acid (1.8:1.0:0.1, v/v/v) as the developing system followed by densitometric scanning at 220 nm. In the HPLC-UV method, the separation was performed using isocratic elution system with acetonitrile: 0.15% triethylamine (pH 2.2) (50:50, v/v) on C18 analytical column. The flow rate was optimized at 1.0 mL·min-1 and UV detection was achieved at 220 nm. Validation was performed in accordance with the International Conference on Harmonization guidelines and the method was perfectly applied for determination of LOX in its pharmaceutical preparation. The results obtained were statistically compared to those obtained after application of the official HPLC method, where no significant difference was found incompliance with precision and accuracy. Identification and characterization of the possible hydrolytic degradation product under alkaline conditions and that produced during oxidative degradation using hydrogen peroxide were structurally elucidated using infrared and mass spectrometry analyses.

Authors+Show Affiliations

Department of Analytical Chemistry, Faculty of Pharmacy, Egyptian Russian University, Cairo, Egypt.Memphis Co. for Pharmaceutical and Chemical Industries, Cairo, Egypt.

Pub Type(s)

Journal Article

Language

eng

PubMed ID

27988488

Citation

Eissa, Maya S., and Osama I. Abd El-Sattar. "Identification and Structure Elucidation of Forced Degradation Products of the Novel Propionic Acid Derivative Loxoprofen: Development of Stability-Indicating Chromatographic Methods Validated as Per ICH Guidelines." Journal of Chromatographic Science, vol. 55, no. 4, 2017, pp. 417-428.
Eissa MS, Abd El-Sattar OI. Identification and Structure Elucidation of Forced Degradation Products of the Novel Propionic acid Derivative Loxoprofen: Development of Stability-Indicating Chromatographic Methods Validated as per ICH Guidelines. J Chromatogr Sci. 2017;55(4):417-428.
Eissa, M. S., & Abd El-Sattar, O. I. (2017). Identification and Structure Elucidation of Forced Degradation Products of the Novel Propionic acid Derivative Loxoprofen: Development of Stability-Indicating Chromatographic Methods Validated as per ICH Guidelines. Journal of Chromatographic Science, 55(4), pp. 417-428. doi:10.1093/chromsci/bmw196.
Eissa MS, Abd El-Sattar OI. Identification and Structure Elucidation of Forced Degradation Products of the Novel Propionic Acid Derivative Loxoprofen: Development of Stability-Indicating Chromatographic Methods Validated as Per ICH Guidelines. J Chromatogr Sci. 2017 Apr 1;55(4):417-428. PubMed PMID: 27988488.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Identification and Structure Elucidation of Forced Degradation Products of the Novel Propionic acid Derivative Loxoprofen: Development of Stability-Indicating Chromatographic Methods Validated as per ICH Guidelines. AU - Eissa,Maya S, AU - Abd El-Sattar,Osama I, PY - 2015/07/23/received PY - 2016/11/29/accepted PY - 2016/12/19/pubmed PY - 2018/3/6/medline PY - 2016/12/19/entrez SP - 417 EP - 428 JF - Journal of chromatographic science JO - J Chromatogr Sci VL - 55 IS - 4 N2 - Loxoprofen sodium (LOX) is a recently developed novel propionic acid derivative. Owing to its instability under both hydrolytic and oxidative conditions, the development of simple, rapid and sensitive methods for its determination in the presence of its possible forced degradation products becomes essential. Two simple chromatographic methods, high-performance thin layer chromatography (HPTLC) and high-performance liquid chromatography (HPLC), were developed associated with ultraviolet (UV) detection. In HPTLC-densitometric method, the separation of LOX from its degradation products was achieved using silica gel F254 plates and toluene:acetone:acetic acid (1.8:1.0:0.1, v/v/v) as the developing system followed by densitometric scanning at 220 nm. In the HPLC-UV method, the separation was performed using isocratic elution system with acetonitrile: 0.15% triethylamine (pH 2.2) (50:50, v/v) on C18 analytical column. The flow rate was optimized at 1.0 mL·min-1 and UV detection was achieved at 220 nm. Validation was performed in accordance with the International Conference on Harmonization guidelines and the method was perfectly applied for determination of LOX in its pharmaceutical preparation. The results obtained were statistically compared to those obtained after application of the official HPLC method, where no significant difference was found incompliance with precision and accuracy. Identification and characterization of the possible hydrolytic degradation product under alkaline conditions and that produced during oxidative degradation using hydrogen peroxide were structurally elucidated using infrared and mass spectrometry analyses. SN - 1945-239X UR - https://www.unboundmedicine.com/medline/citation/27988488/Identification_and_Structure_Elucidation_of_Forced_Degradation_Products_of_the_Novel_Propionic_acid_Derivative_Loxoprofen:_Development_of_Stability_Indicating_Chromatographic_Methods_Validated_as_per_ICH_Guidelines_ L2 - https://academic.oup.com/chromsci/article-lookup/doi/10.1093/chromsci/bmw196 DB - PRIME DP - Unbound Medicine ER -