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Development of the HPLC Method for Simultaneous Determination of Lidocaine Hydrochloride and Tribenoside Along with Their Impurities Supported by the QSRR Approach.

Plenis A, Konieczna L, Miękus N, Bączek T - Chromatographia (2012)

Bottom Line: Intra- and inter-day precision was below 1.97 %, whereas accuracy for all analytes ranged from 98.17 to 101.94 %.Moreover, a comparative study of the RP-LC column classification based on the quantitative structure-retention relationships (QSRR) and column selectivity obtained in real pharmaceutical analysis was innovatively applied using factor analysis (FA).Hence, it was concluded that the proposed QSRR approach could be considered a supportive tool in the selection of the suitable column for the pharmaceutical analysis.

View Article: PubMed Central - PubMed

Affiliation: Department of Pharmaceutical Chemistry, Medical University of Gdańsk, Hallera 107, 80-416 Gdańsk, Poland.

ABSTRACT
A new liquid chromatographic (LC) method for simultaneous determination of lidocaine hydrochloride (LH) and tribenoside (TR) along with their related compounds in pharmaceutical preparations is described. Satisfactory LC separation of all analytes after the liquid-liquid extraction (LLE) procedure with ethanol was performed on a C18 column using a gradient elution of a mixture of acetonitrile and 0.1 % orthophosphoric acid as the mobile phase. The procedure was validated according to the ICH guidelines. The limits of detection (LOD) and quantification (LOQ) were 4.36 and 13.21 μg mL(-1) for LH, 7.60 and 23.04 μg mL(-1) for TR, and below 0.11 and 0.33 μg mL(-1) for their impurities, respectively. Intra- and inter-day precision was below 1.97 %, whereas accuracy for all analytes ranged from 98.17 to 101.94 %. The proposed method was sensitive, robust, and specific allowing reliable simultaneous quantification of all mentioned compounds. Moreover, a comparative study of the RP-LC column classification based on the quantitative structure-retention relationships (QSRR) and column selectivity obtained in real pharmaceutical analysis was innovatively applied using factor analysis (FA). In the column performance test, the analysis of LH and TR in the presence of their impurities was carried out according to the developed method with the use of 12 RP-LC stationary phases previously tested under the QSRR conditions. The obtained results confirmed that the classes of the stationary phases selected in accordance with the QSRR models provided comparable separation for LH, TR, and their impurities. Hence, it was concluded that the proposed QSRR approach could be considered a supportive tool in the selection of the suitable column for the pharmaceutical analysis.

No MeSH data available.


Related in: MedlinePlus

A three-dimensional FA plot for variables (a) and objects (b) based on the regression coefficients of a2, a2′, a3′, and a4′ determined in two QSRR models for 12 RP-LC columns tested
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Fig2: A three-dimensional FA plot for variables (a) and objects (b) based on the regression coefficients of a2, a2′, a3′, and a4′ determined in two QSRR models for 12 RP-LC columns tested

Mentions: The theoretical QSRR results for the 12 stationary phases and their application in pharmaceutical practice for separation of LH and TR along with their impurities were subject to a comparative study to check whether the QSRR approach could be considered a useful tool facilitating the selection of the RP-LC column. An assay employing factor analysis (FA) based on the varimax criterion was conducted to visualise the relationships between the theoretical and practical data sets. The analysis was performed on the Statistica 9.0 software (StatSoft, Tulsa, USA). The FA was first conducted based on the regression coefficients of the QSRR models: a2 from Eq.  1(Table 3) and a2′, a3′, and a4′ from Eq. 2 (Table 4) established for all columns. The obtained FA plots picturing the variables and the objects (columns) in three-dimensional space are shown on Fig. 2a, b, respectively. Then, the retention parameters of the tR and Rs for LH, TR and their impurities (Table 5), calculated for all stationary phases during the column performance test were evaluated by the FA. The three-dimensional plots for the variables and columns resulting from the FA are shown in Fig. 3a, b, respectively. In the calculation, the numbers assigned to the tested columns were the same as those reported in Tables 3, 4, 5.Fig. 2


Development of the HPLC Method for Simultaneous Determination of Lidocaine Hydrochloride and Tribenoside Along with Their Impurities Supported by the QSRR Approach.

Plenis A, Konieczna L, Miękus N, Bączek T - Chromatographia (2012)

A three-dimensional FA plot for variables (a) and objects (b) based on the regression coefficients of a2, a2′, a3′, and a4′ determined in two QSRR models for 12 RP-LC columns tested
© Copyright Policy
Related In: Results  -  Collection

Show All Figures
getmorefigures.php?uid=PMC3585984&req=5

Fig2: A three-dimensional FA plot for variables (a) and objects (b) based on the regression coefficients of a2, a2′, a3′, and a4′ determined in two QSRR models for 12 RP-LC columns tested
Mentions: The theoretical QSRR results for the 12 stationary phases and their application in pharmaceutical practice for separation of LH and TR along with their impurities were subject to a comparative study to check whether the QSRR approach could be considered a useful tool facilitating the selection of the RP-LC column. An assay employing factor analysis (FA) based on the varimax criterion was conducted to visualise the relationships between the theoretical and practical data sets. The analysis was performed on the Statistica 9.0 software (StatSoft, Tulsa, USA). The FA was first conducted based on the regression coefficients of the QSRR models: a2 from Eq.  1(Table 3) and a2′, a3′, and a4′ from Eq. 2 (Table 4) established for all columns. The obtained FA plots picturing the variables and the objects (columns) in three-dimensional space are shown on Fig. 2a, b, respectively. Then, the retention parameters of the tR and Rs for LH, TR and their impurities (Table 5), calculated for all stationary phases during the column performance test were evaluated by the FA. The three-dimensional plots for the variables and columns resulting from the FA are shown in Fig. 3a, b, respectively. In the calculation, the numbers assigned to the tested columns were the same as those reported in Tables 3, 4, 5.Fig. 2

Bottom Line: Intra- and inter-day precision was below 1.97 %, whereas accuracy for all analytes ranged from 98.17 to 101.94 %.Moreover, a comparative study of the RP-LC column classification based on the quantitative structure-retention relationships (QSRR) and column selectivity obtained in real pharmaceutical analysis was innovatively applied using factor analysis (FA).Hence, it was concluded that the proposed QSRR approach could be considered a supportive tool in the selection of the suitable column for the pharmaceutical analysis.

View Article: PubMed Central - PubMed

Affiliation: Department of Pharmaceutical Chemistry, Medical University of Gdańsk, Hallera 107, 80-416 Gdańsk, Poland.

ABSTRACT
A new liquid chromatographic (LC) method for simultaneous determination of lidocaine hydrochloride (LH) and tribenoside (TR) along with their related compounds in pharmaceutical preparations is described. Satisfactory LC separation of all analytes after the liquid-liquid extraction (LLE) procedure with ethanol was performed on a C18 column using a gradient elution of a mixture of acetonitrile and 0.1 % orthophosphoric acid as the mobile phase. The procedure was validated according to the ICH guidelines. The limits of detection (LOD) and quantification (LOQ) were 4.36 and 13.21 μg mL(-1) for LH, 7.60 and 23.04 μg mL(-1) for TR, and below 0.11 and 0.33 μg mL(-1) for their impurities, respectively. Intra- and inter-day precision was below 1.97 %, whereas accuracy for all analytes ranged from 98.17 to 101.94 %. The proposed method was sensitive, robust, and specific allowing reliable simultaneous quantification of all mentioned compounds. Moreover, a comparative study of the RP-LC column classification based on the quantitative structure-retention relationships (QSRR) and column selectivity obtained in real pharmaceutical analysis was innovatively applied using factor analysis (FA). In the column performance test, the analysis of LH and TR in the presence of their impurities was carried out according to the developed method with the use of 12 RP-LC stationary phases previously tested under the QSRR conditions. The obtained results confirmed that the classes of the stationary phases selected in accordance with the QSRR models provided comparable separation for LH, TR, and their impurities. Hence, it was concluded that the proposed QSRR approach could be considered a supportive tool in the selection of the suitable column for the pharmaceutical analysis.

No MeSH data available.


Related in: MedlinePlus