A novel validated UPLC method for quantitation of lopinavir and ritonavir in bulk drug and pharmaceutical formulation with its impurities

Abstract

A simple gradient Ultra Performance liquid chromatographic method (UPLC) was developed for determination of lopinavir and ritonavir from its related impurities and assay for the first time. This method involves the use of a C18 (Acquity UPLC BEH C18, 50 × 2.1 mm, 1.7 µm) column thermostated at 30 o C using triethylamine (pH 2.2): 0.1% H 3 PO 4 in acetonitrile and methanol (85:15) as mobile phase in gradient elution mode. A Photo Diode Array (PDA) detector set at 215 nm was used for detection with flow rate 0.4 mL/min. This method was validated over the range of limit of quantitation (LOQ) to 50 to 150% of impurity specification limit and of working concentration for assay. The developed method was validated for linearity, range, precision, accuracy and specificity. This method was successfully applied for content determination of lopinavir and ritonavir in pharmaceutical formulations. This method can be conveniently used in quality control laboratory for routine analysis for assay and related substances as well as for evaluation of stability samples of bulk drugs and pharmaceutical formulations.Uniterms: Lopinavir/determination. Ritonavir/determination.Ultra Performance liquid chromatography/ qualitative analysis.Ultra Performance liquid chromatography/quantitative analysis. Bulk drugs/qualitative analysis. Pharmaceutical formulations/qualitative analysis. Pharmaceutical formulations/impurity profile. Bulk drugs/impurity profile.Desenvolveu-se, pela primeira vez, método de cromatografia líquida de ultra-eficiência (UPLC), com gradiente simples, para a determinação de lopinavir e ritonavir e suas impurezas relativas. Esse método envolve o uso de C18 (Acquity UPLC BEH C18, 50 × 2,1 mm, 1,7 µm), termostatizada a 30 o C, utilizandose trietilamina (pH 2,2) e fase móvel de H 3 PO 4 0,1% em acetonitrila e metanol (85:15), em eluição por gradiente. Detector de arranjo de fotodiiodo (PDA), fixado a 215 nm, foi utilizado para a detecção, com fluxo de 0,4 mL/min. Esse método foi validado em faixa de limite de quantificação (LOQ) de 50 a 150% de limite de impureza e da concentração de trabalho para o ensaio. O método desenvolvido foi validado quanto à linearidade, faixa, precisão, exatidão e especificidade. Esse método foi aplicado com sucesso para a determinação de lopinavir e de ritonavir em formulações farmacêuticas. Tal método pode ser convenientemente utilizado em laboratório de controle de qualidade, não só para análise de rotina e ensaio de substâncias relacionadas, como também para a avaliação da estabilidade de amostras a granel ou em formulações farmacêuticas.Unitermos: Lopinavir/determinação. Ritonavir/determinação. Cromatografia Líquida de Ultra Eficiência/ análise qualitativa.Cromatografia Líquida de Ultra Eficiência/análise quantitativa. Fármacos a granel/ análise qualitativa. Formulações farmacêuticas/análise qualitativa.Formulações farmacêuticas/perfil de impureza. Fármacos a granel/perfil de impureza. INTRODUCTIONLopinavir is an anti-Human immunodeficiency virus (HIV) drug which belongs to the class of drug...

Simultaneous determination of newly developed antiviral agents in pharmaceutical formulations by HPLC-DAD

“…A review of the literature revealed that CE [15, 16], HPLC [17–21], UPLC–MS/MS [22–24], LC–MS/MS [25, 26] and HPTLC [27, 28] methods have been reported for the analysis of RIT, individually or in combination with other drugs. However, a method for the simultaneous determination of OMB, PAR, RIT and DAS has not yet been reported.…”

An Inclusive Review on Analytical Methods for Ritonavir in Various Pharmaceutical and Biological Matrix

“…Quantitation was performed with photo Diode Array (PDA) detector at 215 nm with flow rate 0.4 mL/min. 22…”

Combining subsidiary and synchronous approaches for concurrent spectrofluorimetric assurance of lopinavir and ritonavir in tablets utilized in convention for treatment of coronavirus infection (COVID-19) and biological fluids

“…Ritonavir was decided alone or in combinations by assortment of strategies as electrochemical strategies [11] , spectrophotometry [12] , [13] , [14] , HPLC [15] , [16] , [17] , TLC-densitometry [18] , [19] , [20] and LC-MS [21] , [22] , [23] , [24] . There are detailed strategies for the assurance of the two drugs together either in their twofold blend or within the nearness of other antiviral drugs as spectrophotometry [25] , [26] , [27] , HPLC [28] , [29] , [30] , [31] , TLC-densitometry [32] , [33] , [34] and LC-MS [35] , [36] , [37] , [38] . There’s no reported detailed strategy for the assurance of the two drugs together either in their twofold blend or within the nearness of their debasement items by synchronous spectrofluimetry.…”