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Spectrophotometric and chromatographic simultaneous estimation of amitriptyline hydrochloride and chlordiazepoxide in tablet dosage forms.

Patel S, Patel NJ - Indian J Pharm Sci (2009)

Bottom Line: The separation was carried out on Merck thin layer chromatographic aluminium sheets of silica gel 60 F254 using carbon tetrachloride: acetone: triethylamine (6:3:0.2, v/v/v) as mobile phase.The linearity was found to be in the range of 50-600 and 20-240 ng/spot for amitriptyline hydrochloride and chlordiazepoxide, respectively.The methods were successively applied to pharmaceutical formulation because no chromatographic interferences from the tablet excipients were found.

View Article: PubMed Central - PubMed

Affiliation: S. K. Patel College of Pharmaceutical Education and Research, Department of Pharmaceutical Chemistry, Ganpat University, Kherva, Mehsana-382711, Gujarat, India.

ABSTRACT
A binary mixture of amitriptyline HCl and chlordiazepoxide was determined by three different methods. The first method involved determination of amitriptyline HCl and chlordiazepoxide using the first derivative spectrophotometric technique at 219 and 230 nm over the concentration ranges of 1-20 and 2-24 mug/ml with mean accuracies 100.9+/-0.87 and 99.2+/-1.0%, respectively. The second method was reversed-phase high performance liquid chromatography using methanol: acetonitrile: 0.065 M ammonium acetate buffer (50:20:30, v/v/v), final pH adjust to 5.5 +/- 0.02 with ortho phosphoric acid as the mobile phase and was pumped at a flow rate of 1.0 ml/min. Quantification was achieved with ultraviolet detection at 240 nm over concentration ranges of 0.25-4 and 0.1-1.6 mug/ml; mean accuracies were 100.55+/-0.62 and 100.71+/-0.81%, respectively. The third method utilized high performance thin layer chromatography method in tablet dosage form. The method was based on separation of the two drugs followed by densitometric measurements of their spots at 240 nm. The separation was carried out on Merck thin layer chromatographic aluminium sheets of silica gel 60 F254 using carbon tetrachloride: acetone: triethylamine (6:3:0.2, v/v/v) as mobile phase. The linearity was found to be in the range of 50-600 and 20-240 ng/spot for amitriptyline hydrochloride and chlordiazepoxide, respectively. The methods were successively applied to pharmaceutical formulation because no chromatographic interferences from the tablet excipients were found. The suitability of these methods for the quantitative determination of the compounds was proved by validation.

No MeSH data available.


Related in: MedlinePlus

RP-HPLC chromatogram of AMI and CLR at 240 nm. AMI is amitriptyline HCl and CLR is chlordiazepoxide
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Figure 0002: RP-HPLC chromatogram of AMI and CLR at 240 nm. AMI is amitriptyline HCl and CLR is chlordiazepoxide

Mentions: To optimize the proposed RP-HPLC method, different systems were tried for chromatographic separation of the two components by combining homogenous design and solvent polarity optimization. The best resolution was achieved using a mobile phase consisting of methanol:acetonitrile:0.065 M ammonium acetate buffer (50:20:30, v/v/v) and final pH adjust to 5.5±0.02 with phosphoric acid, which even gave good sensitivity for both drugs (fig. 2). System suitability testing of the RP-HPLC method gave good relative retention time= 1.83; theoretical plates= 4640.66 and 6960; asymmetry factor (A)= 0.91 and 0.93; tailing factor (T)= 0.96 and 0.97 for AMI and CLR, respectively (Table 1). A linear relation was obtained between peak area and the concentration of the two drugs in the range of 0.25-4 and 0.1-1.6 μg/ml for AMI and CLR, respectively. The linear regression Eqns were, Y= 517021X−31721, r= 0.9999 and Y=1000000 X– 8895.6, r= 0.9997, where Y is the area under the peak, X is the concentration in μg/ml, and r is the correlation coefficient.


Spectrophotometric and chromatographic simultaneous estimation of amitriptyline hydrochloride and chlordiazepoxide in tablet dosage forms.

Patel S, Patel NJ - Indian J Pharm Sci (2009)

RP-HPLC chromatogram of AMI and CLR at 240 nm. AMI is amitriptyline HCl and CLR is chlordiazepoxide
© Copyright Policy - open-access
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC2865828&req=5

Figure 0002: RP-HPLC chromatogram of AMI and CLR at 240 nm. AMI is amitriptyline HCl and CLR is chlordiazepoxide
Mentions: To optimize the proposed RP-HPLC method, different systems were tried for chromatographic separation of the two components by combining homogenous design and solvent polarity optimization. The best resolution was achieved using a mobile phase consisting of methanol:acetonitrile:0.065 M ammonium acetate buffer (50:20:30, v/v/v) and final pH adjust to 5.5±0.02 with phosphoric acid, which even gave good sensitivity for both drugs (fig. 2). System suitability testing of the RP-HPLC method gave good relative retention time= 1.83; theoretical plates= 4640.66 and 6960; asymmetry factor (A)= 0.91 and 0.93; tailing factor (T)= 0.96 and 0.97 for AMI and CLR, respectively (Table 1). A linear relation was obtained between peak area and the concentration of the two drugs in the range of 0.25-4 and 0.1-1.6 μg/ml for AMI and CLR, respectively. The linear regression Eqns were, Y= 517021X−31721, r= 0.9999 and Y=1000000 X– 8895.6, r= 0.9997, where Y is the area under the peak, X is the concentration in μg/ml, and r is the correlation coefficient.

Bottom Line: The separation was carried out on Merck thin layer chromatographic aluminium sheets of silica gel 60 F254 using carbon tetrachloride: acetone: triethylamine (6:3:0.2, v/v/v) as mobile phase.The linearity was found to be in the range of 50-600 and 20-240 ng/spot for amitriptyline hydrochloride and chlordiazepoxide, respectively.The methods were successively applied to pharmaceutical formulation because no chromatographic interferences from the tablet excipients were found.

View Article: PubMed Central - PubMed

Affiliation: S. K. Patel College of Pharmaceutical Education and Research, Department of Pharmaceutical Chemistry, Ganpat University, Kherva, Mehsana-382711, Gujarat, India.

ABSTRACT
A binary mixture of amitriptyline HCl and chlordiazepoxide was determined by three different methods. The first method involved determination of amitriptyline HCl and chlordiazepoxide using the first derivative spectrophotometric technique at 219 and 230 nm over the concentration ranges of 1-20 and 2-24 mug/ml with mean accuracies 100.9+/-0.87 and 99.2+/-1.0%, respectively. The second method was reversed-phase high performance liquid chromatography using methanol: acetonitrile: 0.065 M ammonium acetate buffer (50:20:30, v/v/v), final pH adjust to 5.5 +/- 0.02 with ortho phosphoric acid as the mobile phase and was pumped at a flow rate of 1.0 ml/min. Quantification was achieved with ultraviolet detection at 240 nm over concentration ranges of 0.25-4 and 0.1-1.6 mug/ml; mean accuracies were 100.55+/-0.62 and 100.71+/-0.81%, respectively. The third method utilized high performance thin layer chromatography method in tablet dosage form. The method was based on separation of the two drugs followed by densitometric measurements of their spots at 240 nm. The separation was carried out on Merck thin layer chromatographic aluminium sheets of silica gel 60 F254 using carbon tetrachloride: acetone: triethylamine (6:3:0.2, v/v/v) as mobile phase. The linearity was found to be in the range of 50-600 and 20-240 ng/spot for amitriptyline hydrochloride and chlordiazepoxide, respectively. The methods were successively applied to pharmaceutical formulation because no chromatographic interferences from the tablet excipients were found. The suitability of these methods for the quantitative determination of the compounds was proved by validation.

No MeSH data available.


Related in: MedlinePlus