التقدير الكروماتوغرافي والطيفي لبعض الأدوية المضادة للاكتئاب

Chromatographic and spectrophotometric determination of some antidepressant drugs

Abstract

The work (the thesis) consisted of two main parts,:
“-The first part”: high-performance reverse-phase liquid chromatography (Rp-HPLC).
The first part: Reversible phase Liquid Chromatography”Rp-HPLC
This method was developed to be accurate, sensitive and rapid for estimation Chlordiazepoxide , Diazepam , Amitriptyline , and Alprazolam drugs , in their alone state and as a combination,”were separated using an”analytical column type”)the ODS2-C18 (250 mm × 4.6 mm × 5μm particle”) at 35°C, and at a flow rate of 1.0 ml/min using the Isocratic system for the mobile phase. The mobile phase used included a solution of disodium phosphate ions with two organic axes are: methanol and acetonitrile with a ratio (40:30:30 v/v)) and an pH = 4, using a UV detector at a wavelength of 241nm”. “The retention time for chlordiazepoxide was 5.123 minخ, 2.753 min” ,for diazepam, 3.426 min( , for amitriptyline ة, and 3.703 minutes for<alprazolam. The method was evaluated from calculating the linearity )5-50)) µg (/) ml and correlation coefficient (R2 = 0.9988) and (6-48) µg: / ml (10-50) and (R2 = 0.9997) and R2=0.9996) and R2=0.9982) for chlordiazepoxide, diazepam, alprazolam and amitriptyline, respectively, . the relative standard deviation of both drugs was less than 2%, with the lowest detection limits (0.634 , 0.616 , 0.77 0.72 ) µg/mL for chlordiazepoxide, diazepam, amitriptyline, and alprazolam ,(respectively). The limits of Quantitative detection (1.922, 1.868 , 2.57 , 2.50) µg/ml for chlordiazepoxide, diazepam, amitriptyline, and alprazolam. The chromatographic method was applied to pharmaceutical preparations in their pure form and in their pharmaceutical preparations, and the recoveries were within (99.207-102.544) %, (99.046-100.858%), (100.29-100.51%) (99.95-101.12%) for chlordiazepoxide, diazepam, alprazolam and amitriptyline, respectively.

The second part:

The spectroscopic method (oxidation-reduction method)
An accurate, sensitive and simple the spectral method was developed, using oxidation reduction reactions, which included the determination of some psychotropic drugs in the first paragraph, including chlordiazepoxide, diazepam, alprazolam and amitriptyline for quantitative determination in its pure form and in pharmaceutical preparations.
ا The method included the determination of each drug individually by reacting it with the reagent 3-methyl-2-benzothiazole non-hydrazine hydrochloride hydrate in the presence of the oxidizing agent and iron(III) chloride in a strong acidic medium. Preliminary tests were conducted to determine the appropriate conditions to obtain sensitivity. The maximum wavelength of the formed colored complex”was”measured”as)(AM=630.0nm,663.0nm=CH,619.0nm=ALP,609.0 nm=DIZE).{the optimum conditions were also studied to obtain the highest absorbance intensity. Beer’s law limits were within the concentration range (5-30) μg /ml for diazepam, alprazolam or amitriptyline(2-30) μg /ml, either chlordiazepoxide (5-25) μg / ml and with the correlation coefficient for each drug alprazolam, amitriptyline, diazepam and chlordiazepoxide (0.9979,0.9965,0.9995,0.9997) on the straight, and through the values of the molar absorption coefficient and Sandal’s sensitivity to the “formed” matrix, which were equal to (5.575 x 103, 3.359 x 103, 7.565 x 103 and (7.157 x 103 L/mol.cm) 0.054, 0.085, 0.041, 0.039 (µg/cm2), respectively, The method showed high sensitivity. The relative standard deviation for each drug was less than 2%, the detection limits for drugs are )0.877, 0.739, 1.779 and (1.757( µg/ml, and the quantitative limits are 2.924, 2.464, 5.930, 5.857) µg/ml for chlordiazepoxide, diazepam, alprazolam and amitriptyline. through the mentioned results, this method has high accuracy and precision, and therefore it has been applied in estimating these drugs in their pure state and in their pharmaceutical preparations.