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offf222222����Utility of Acid Dyes for Tramadol Determination in Pure and in Dosage Forms Spectrophotometrically

Alaa S. Amin,1,* Ahmed M. Adawy2, and Ghada M. Doma1 

1 Chemistry Department, Faculty of Science, Benha University, Benha, Egypt
2 Forensic Chem. lab, Forensic Medicine Authority, Ministry of Justice, Egypt

Abstract
Simple, rapid, and extractive spectrophotometric methods were developed for the determination of tramadol hydrochloride in pure and in dosage forms. These methods are based on the formation of ion-pair complexes between the basic drug and acid dyes, namely, Eriochrome black T (EBT), Alizarin red S (ARS), Cresol red (CR), and Phenol red (PR) in acidic media. The formed complexes were extracted with methylene chloride and measured at 513, 430, 400, and 400 nm for EBT, ARS, CR, and PR, respectively. The analytical parameters and their effects are optimized and investigated. Beer�s law was obeyed in the ranges 1.0�11 �g/ml using EBT, whereas 1-10 �g/ml on using ARS, CR, and PR, respectively, was obtained. The molar absorptivity was calculated to be 5.10 � 104, 7.7 � 103, 7.4 � 103 and 3.1 � 104 l mol"1 cm"1 on using EBT, ARS, CR, and PR, respectively. Sandell sensitivity was found as 1.8, 0.38, 0.41, and 0.96 ng cm"2, respectively. The proposed methods have been applied successfully for the analysis of tramadol hydrochloride in pure forms and pharmaceutical formulations. Statistical comparison of the results with the reference methods showed excellent agreement and indicated no significant difference in accuracy and precision.


*Corresponding author. Tel.: +20 552350996; fax: +20 133222578;  
E-mail address:  HYPERLINK "mailto:asamin2005@hotmail.com" asamin2005@hotmail.com.
Keywords Tramadol determination; Spectrophotometry; Ion pair complexation; Pharmaceutical formulations.

Introduction
Tramadol hydrochloride ((�) trans-2-[(dimethylamino)methyl]-1-(3-methoxy-phenyl)-cyclohexanol) is a synthetic, centrally acting, analgesic agent (Fig. 1), used for the relief of moderate to chronic pain and has no clinically relevant cardiovascular or respiratory depressant activity. Furthermore, it does not have a prostaglandin inhibitory effect. The racemate is successfully used for the treatment of severe postoperative or cancer pains. The dosage of tramadol should be adjusted to the intensity of pain and to the response of an individual patient [1�3]. (Its therapeutic plasma concentration is in the range of 100�300 ng/l. Tramadol is rapidly and almost completely absorbed after oral administration but its absolute bioavailability is only 65�70% due to first-pass metabolism. Approximately 10�30% of the parent drug is excreted unmetabolised in the urine [4,5]. Determination of tramadol in biological samples involves an initial sample pretreatment step for isolation of target analytes, using liquid�liquid extraction (LLE) [6�11] and solid phase extraction (SPE) [12,13] techniques, prior to high performance liquid chromatography (HPLC). But these techniques have many disadvantages as they are tedious, labor intensive, time consuming and very prone to loss of analyte. 


Fig. 1 Structure of Tramadol Hydrochloride

Literature survey reveals that, several spectrophotometric method [14-16] TLC- densitometry [17], UV spectrophotometric and HPLC-DAD methods [18], HPLC method [19-23] High Performance thin layer chromatography-densitometry [24], GC [25], capillary electrophoresis [26], voltammetry [27] and potentiometry [28], have been reported for the estimation of tramadol in pharmaceutical formulations. Few analytical methods were reported in literature for the determination of tramadol and other combination drugs which includes spectrophotometric method [29�35], spectrophotometric and spectrofluorimetric method [36].
The spectrophotometric technique continues to be the most preferred method for the assay of different classes of drugs in pure, pharmaceutical formulations and in biological samples, for its simplicity and reasonable sensitivity with significant economical advantages. Spectrophotometric methods are reported for the assay of tramadol [29�35]. These methods were associated with some major drawbacks such as decreased selectivity due to measurement in ultraviolet region and/or decreased simplicity of the assay procedure (e.g., tedious precipitation, heating, or liquid-liquid extraction steps in the ion pair formation-based methods). For these reasons, it was worthwhile to develop a new simple and selective spectrophotometric method for the determination of the studied drugs in their pharmaceutical dosage forms.
In the present work, the development of accurate and precise extractive spectrophotometric methods were reported based on the methylene chloride soluble ion-pair complexes between tramadol and some acid dyes (EBT, ARS, CR, and PR). The absorbance measurements were measured at optimum wavelengths. The proposed methods were applied successfully for the determination of tramadol in pure and dosage forms. No interference was observed from the additives. The methods provide rapid, economic procedures and more sensitive compared to the previously reported spectrophotometric methods. These methods were validated by the statistical data.

Materials and methods
Apparatus 
All absorption spectra were made using JASCO V-670 UV/Vis spectrophotometer (Japan) with a scanning speed of 200 nm/min and a band width of 2.0 nm, equipped with 10 mm matched quartz cells. 

Materials and reagents 
All the solutions were freshly prepared. All solvents and chemicals used in this study were of analytical grade quality of the highest purity and used without further purification.
 Eriochrome black T (EBT), Alizarin red S (ARS), Cresol red (CR), and Phenol red (PR) (BDH Chemicals Ltd., Poole, England) were used without further purification. Stock solutions (5.0 � 10"3 M) of reagents were prepared by dissolving the appropriate weight of each reagent in 10 ml of methanol and diluted to 100 ml with bidistilled water. These solutions are stable for at least one week if kept in the refrigerator.
Tramadol hydrochloride (raw material) was obtained from Memphis Pharmaceutical & Chemical Industries, Egypt. A standard stock solution containing 1.0 mg/ml was prepared by dissolving 100 mg of tramadol hydrochloride in 100 ml of distilled water. From this, a working standard solution containing 100 �g/ml was prepared for the proposed method.
Hydrochloric acid Solution of 0.01 M was prepared by transferring 8.28 ml of concentrated solution of the acid, Riedel-de-Haen AG-Germany (12.07 M), to 1000 ml measuring flask and diluted to the mark with distilled water.

General procedures
Aliquots of (0.1 1.1 ml) the standard drug solution (100 �g mL"1) were transferred to 10 ml measuring flasks and added 0.5 ml of 0.01 M HCl on using EBT and/or 0.1 ml of 0.01 M HCl on using ARS, CR, and PR, and then added 3.0 ml of EBT and PR and/or 2.0 ml of 5.0 � 10"3 M ARS and CR. The mixture was extracted with 10 ml (3 � 3 ml) methylene chloride by shaking for 2.0 min and then allowed to stand for clear separation of phase and the methylene chloride layer was passed through anhydrous sodium sulphate. The absorbance of the yellow colored complexes was measured at 513, 430, 400, and 400 nm, using EBT, ARS, CR, and PR., respectively, against corresponding reagent blank similarly prepared. All measurements were made at room temperature (25 � 2 �C). The procedures were repeated for other analyte aliquots and calibration plots were drawn to calculate the amount of drugs in unknown analyte samples.

Applications to pharmaceutical formulations  
A- Assay for tablets (Tamol-x). 
Twenty tablets of tramadol hydrochloride were accurately weighed and powdered. Tablet powder equivalent to 100 mg of tramadol hydrochloride was dissolved in 50 ml of distilled water, sonicated for 15 min, filtered and washed with distilled water. The filtrate and washings were combined and the final volume was made to 100 ml with distilled water. The solution was suitably diluted and analyzed as given under the assay procedure for bulk samples. None of the excipients usually employed in the formulation of tablets interfered in the analysis of tramadol hydrochloride, by the proposed methods.

B- Assay for capsules (Tramajak 100 mg)
A quantity of powder equivalent to 25 mg of Tramadol Hydrochloride was taken in a 25 ml volumetric flask and it was first dissolved in 2.5 ml of N-N-dimethylformamide by shaking the flask for 3.0 to 5.0 min and diluted up to the mark with distilled water. Then the solution was filtered using Whatmann filter paper No.40. From this filtrate, appropriate dilutions were made with distilled water to obtain the desired concentration (90, 120 and 150 �g/ml). 


C- Assay for ampoules (TRAM, 100 mg/2.0 ml)
The content of five ampoules of TRAM (100 mg/2.0 ml) (Manufactured by Misr Pharmaceuticals Co., Egypt) was mixed and the average volume of one ampoule was determined. Accurately measured volume equivalent to 20 mg of tramadol was transferred into a 100 ml measuring flask and diluted to the mark with distilled water. Suitable dilution was made to fit the applicable concentration range and the above described procedures were followed. The nominal content of the ampoules was calculated either from calibration graph or using the regression equation.

Stoichiometric relationship 
The stoichiometric ratios of the ion-associates formed between the tramadol under investigation and the reagents were determined by applying the continuous variation [37] and the molar ratio [38] methods at the wavelengths of maximum absorbance. In continuous variation method, equimolar solutions were employed: 5.0 � 10"3 M standard solutions of drug and 5.0 � 10"3 M solutions of dye were used. A series of solutions was prepared in which the total volume of the studied drugs and the dye was kept at 2.0 ml. The drug and reagent were mixed in various complementary proportions (0 : 2, 0.2 : 1.8, 0.4 : 1.6,. . .,2 : 0, inclusive) and completed to volume in a 10 ml calibrated flask with the appropriate solvent for extraction following the above mentioned procedure. In the molar ratio method, the concentrations of tramadol are kept constant (1.0 ml of 5.0 � 10"4 M) while that of dyes (5.0 � 10"4 M) are regularly varied (0.2 2.4 ml). The absorbance of the prepared solutions optimum is measured at optimum condition at wavelength for each complex.




results and discussion

3.1. Absorption Spectra
The nitrogenous drugs are present in positively charged protonated forms and anionic dyes present mainly in anionic form at pH e" 2.5. So when treated with an acid dye at pH range 2.8 4.0 of acidic buffers solutions, a yellow ion-pair complex which is extracted with methylene chloride is formed. The absorption spectra of the ion-pair complexes, which were formed between tramadol, and EBT, ARS, CR, and PR were measured in the range 350�600 nm against the blank solution. The ion-pair complexes of EBT, ARS, CR, and PR show maximum absorbance at 513, 430, 400, and 400 nm, respectively.

Optimum reaction conditions for complex formation
The optimization of the methods was carefully studied to achieve complete reaction formation, highest sensitivity, and maximum absorbance. 

A- Effects of acidity on ion-pair formation
The effect of acidity on the drug-reagent complex was studied by extracting the colored complexes in the presence of various acid media (H2SO4, HCl, HNO3, H3PO4, and CH3COOH). It was noticed that the maximum color intensity and highest absorbance value were observed in 0.01 M HCl in addition to the stability of the color without affecting the absorbance at the optimum acid media. Moreover the amount of 0.01 M HCl was examined for different reagents used (Fig. 2). It was found that 0.5 ml was the optimum on using EBT, whereas 0.1 ml was the best on using ARS, CR, and PR, which gave maximum absorbance and reproducible results. 


B- Effect of extracting solvents 
The effect of several organic solvents, namely, chloroform, carbon tetrachloride, methylene chloride, ethylene chloride, methanol, ethanol, 
 EMBED Origin50.Graph 

Fig. 2  Effect of 0.01 M HCl volume on the complexation
of TRM with the studied reagents

acetonitrile, n-butanol, benzene, acetone, ethyl acetate, diethyl ether, toluene, dichloromethane, and chlorobenzene, was studied for effective extraction of the colored species from aqueous phase. Methylene chloride was found to be the most suitable solvent for extraction of colored ion-pair complexes for all reagents quantitatively. Experimental results indicated that triple (3 � 3 ml) extraction with total volume 10 ml, yielding maximum absorbance intensity, stable absorbance for the studied drug and considerably lower extraction ability for the reagent blank and the shortest time to reach the equilibrium between both phases. 

C- Effects of reagents concentration 
The effect of the reagents was studied by measuring the absorbance of solutions containing a fixed concentration of tramadol and varied amounts of the respective reagents. Maximum color intensity of the complex was achieved with 3.0 ml of 5.0 � 10"3 M of EBT and PR, whereas 2.0 ml of ARS, and CR was sufficient to give highest absorbance for the formed complexes.  A larger volume of reagent had no pronounced effect on the absorbance of the formed ion-pair complex (Fig. 3).
 EMBED Origin50.Graph 

Fig. 3  Effect of reagents on ion-pair complexation with 5.0 �g/ml tramadol

D- Effect of time and temperature
The optimum reaction time was investigated from 0.5 to 5.0 min by following the color development at ambient temperature (25 � 2 �C). Complete color intensity was attained after 2.0 min of mixing for all complexes. The effect of temperature on colored complexes was investigated by measuring the absorbance values at different temperatures. It was found that the colored complexes were stable up to 35 �C. At higher temperatures, the drug concentration was found to increase due to the volatile nature of the methylene chloride. The absorbance remains stable for at least 15 h at room temperature for all reagents.

Stoichiometric relationship
The stoichiometric ratio between drug and dye in the ion-pair complexes was determined by the continuous variations method. Job�s method of continuous variation of equimolar solutions was employed:
a 5.0 � 10"4 M standard solution of drug base and 5.0 � 10"4 M solution of BCG, BCP, BPB, BTB, or MO, respectively, were used. A series of solutions was prepared in which the total volume of drug and reagent was kept at 2.0 ml. The absorbance was measured at the optimum wavelength. The results indicate that 1 : 1 (drug : dye) ion-pairs are formed through the electrostatic attraction between positive protonated tramadol and negative EBT", ARS", CR", and PR". The extraction equilibrium can be represented as follows:

TRM+(aq) + D"(aq) �!�! TRM+D"(aq) �!�! TRM+D"(org),          (1)

Where TRM+ and D" represent the protonated TRM and the anion of the dye, respectively, and the subscripts (aq) and (org) refer to the aqueous and organic phases, respectively.  A representative example for the suggested reaction between Tramadol and EBT is shown in the following mechanism:-





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Conditional stability constants of ion-pair complexes
The stability of the ion-pair complexes was evaluated. The formation of the ion-pair complexes was rapid and the yellow color extracts were stable at least for 15 h for drug-dye without any change in color intensity and with the maximum absorbance at room temperature. The conditional stability constants of the ion-pair complexes for the studied drug were calculated from the continuous variation data using the Harvey and Manning equation [39]:

Method of validation

Linearity
At described experimental conditions for tramadol determination, standard calibration curves with reagents were constructed by plotting absorbance versus concentration. The statistical parameters were given in the regression equation calculated from the calibration graphs. The linearity of calibration graphs was proved by the high values of the correlation coefficient (r2) and the small values of the intercepts of the regression equations. The apparent molar absorptivities of the resulting colored ion-pair complexes and relative standard deviation of response factors for each proposed spectrophotometric method were also calculated and recorded in Table 1. The molar absorptivity of EBT > PR > ARS > CR > BPB ion-pair complexes for tramadol.

Sensitivity 
The limits of detection (LOD) and quantitation (LOQ) for the proposed methods were calculated [39, 40]. In accordance with the formula, the limits of detection for tramadol were found to be 0.288, 0.309, 0.325 and 0.281 �g/ml for EBT, ARS, CR and PR methods, respectively. The limit of quantitation for tramadol was found to be 0.842, 0.939, 0.984, and 0.825 �g/ml, respectively.

Accuracy and precision 
Specificity of ion-pair reaction and selective determination of tramadol, were the basic nitrogenous compounds with acid dyes could be possible. Percentage relative standard deviation (RSD%) as precision and percentage relative error (RE%) as accuracy of the suggested methods were calculated. Precision was carried out by six determinations at four different concentrations in these spectrophotometric methods. The percentage relative error was calculated using the following equation:

RE% = [founded " added/ added] � 100. (2)

The interday and intraday precision and accuracy results are shown in Tables 2. These results of accuracy and precision showed that the proposed methods have good repeatability and reproducibility.




Table 1 Statistical analysis of calibration graphs and analytical data
           in the determination of tramadol using the proposed methods.
ParametersEBTARSCRPRWavelengths  �max (nm)513430400400Acidity (0.01M HCl)0.50.10.10.1Beer s law limits  (�g/ml)1.0 111.0 101.0 101.0 10�,  (l mol"1�cm"1) x 1045.10.740.773.1Sandell sensitivity (ng cm-2)1.8 0.38, 0.41 0.96 log�Kf4.14 4.034.274.08Regression equation aIntercept (a)- 0.002- 0.0003- 0.0048- 0.0024Slope (b)0.170.0260.0250.10Correlation coefficient (r)0.99920.99880.99940.9990LOD (�g/ml) b0.288,  0.309 0.325  0.281 LOQ (�g/ml) b0.842 0.939 0.984 0.825 Mean 
� SD99.35 
�  0.4899.60
 � 0.3999.45 
�  0.7899.15
 �  0.90RSD%0.480.390.780.90RE%0.500.410.820.95t-test c1.170.920.890.99F- test c1.631.421.351.48
a A =�a�+�bC, where C is the concentration in �g/ml, A is the absorbance
b LOD, limit of detection; LOQ, limit of quantification; �, molar absorptivity.
c The theoretical values of t and F at P= 0.05 are 2.57 and 5.05, respectively.




ruggedness was expressed as RSD% of the same procedure applied by two analysts and with two different instruments on different days (Table 3). The results showed no statistical differences between procedures done with different analysts and instruments suggesting that the developed methods were robust and rugged.

Effects of interference 
To assess the usefulness of the methods, the effect of diluents, excipients, and additives often accompany tramadol in their dosage forms (starch, lactose, glucose, sucrose, talc, sodium chloride, titanium dioxide, and magnesium stearate) was studied. The results indicated that there is no interference from excipients and additives, indicating a high selectivity for determining tramadol in its dosage forms.

Analysis of pharmaceutical formulations 
The proposed methods have been successfully applied to the determination of tramadol in pharmaceutical dosage forms. Six replicate determinations were made. Moreover, to check the validity of the proposed methods, dosage forms were tested for possible interference with standard addition method (Table 4). There was no significant difference between slopes of calibration curves and standard addition methods. Therefore it is concluded that the excipients in pharmaceutical dosage forms of tramadol were not found any interference in the analysis. At 95%confidence level the calculated t- and F-values did not exceed the theoretical values indicating no significant difference between the proposed methods and the reported methods tramadol [41]. The results showed that satisfactory recovery data were obtained and the assay results were in good agreement with the reported methods.
 Method Added 
 �g/mlIntra-dayInter-day  Recovery 
%Precision
RSD % a  Accuracy
RE %Confidence
 limit b Recovery 
% Precision
RSD % aAccuracy
RE %Confidence
 limit bEBT2.599.600.560.302.49�0.02499.600.48-0.702.49 � 0.0205.099.200.97-0.404.96�0.101100.400.860.505.02 � 0.0917.5100.271.21-0.507.52�0.20299.731.16-0.307.48�0.194AZR3.0100.330.790.103.01�0.01799.670.68-0.302.99 � 0.0146.099.501.17-0.505.97�0.07399.330.84-0.705.96 � 0.0539.0100.441.280.409.04�0.13599.561.50-0.608.96 � 0.156CR2.099.500.79-0.601.99 �0.016100.000.820.402.00 � 0.0174.099.751.29-0.103.99 �0.10899.001.27-0.503.96 � 0.1066.098.831.58-0.505.93 �0.231100.831.48-0.806.05 � 0.216PR3.399.700.54-0.403.29 �0.023100.610.460.203.32 � 0.0196.699.551.26-0.306.57 � 0.132100.160.94-0.906.61 � 0.0989.999.801.94-0.809.88 �0.323100.41.901.24-0.109.94 �0.208Table 2 Intra-day and Inter-day precision and accuracy data for AMS obtained by the proposed methods.














a Mean of six determination, RSD%, percentage relative standard deviation; RE%, percentage relative error. 
b Confidence limit at 95% confidence level and five degrees of freedom (t = 2.57).
Table 3 Method robustness and ruggedness expressed as intermediate
              precision (RSD %) for TRM-EBT ion pair complex.
AMS taken 
�g/mlRobustnessRuggednessParameters alteredInter-analystsInter-instrumentsVolume of EBT aVolume of buffer bReaction time c(RSD %)
(N=3)(RSD %)
(N=3)2.01.882.152.161.902.206.05.405.705.902.201.701010.259.7810.202.601.80
a The volumes of BCP dye used were 3.0 � 0.2 ml.
b The volumes of buffer used were 0.5 � 0.05 ml.
c The reaction times were 2.0 � 0.5 min.

Conclusion
The proposed spectrophotometric method was found to be simple, sensitive, accurate and precise for determination of tramadol in pure and in dosage form. The method utilizes easily available and cheap solvent for analysis, hence the method was also economic for estimation of tramadol in dosage form. The common excipients and additives are usually present in the combined dosage form do not interfere in the analysis, hence it can be conveniently adopted for routine quality control analysis of the drugs in combined dosage form.







Table 4 Application of the standard addition technique for the determination of TRM in dosage forms using the proposed methods.

Sample  Taken  
�g/ml           EBTAZRCRPROfficial [3]Added
 �g/mlRecoverya
(%)Recovery a
(%)Recovery a
(%)Recovery a
(%)Recovery a
(%)Tamol-x 
tablets
2.0-  99.099.70  99.8099.30101.002.0  99.3098.80  99.9099.70  99.504.0100.4099.20  99.3098.50  98.676.0  99.4099.70101.1099.00101.508.0  99.5099.40  98.4099.20100.67Mean
�RSD %    99.52
 � 0.49   99.36
    � 0.68    99.70
 � 0.88  99.14 
   � 0.82   100.27
� 0.59V0.240.460.770.670.35S.E0.200.280.360.330.24t-value b0.650.110.160.46F-value b1.451.312.201.91Tramajak 100 mg3.0-  99.33101.00100.67  99.00  98.671.5100.25  99.67  99.50100.87100.673.0100.67  99.00100.50  99.50101.004.5  99.67101.33  99.00101.25  99.506.0  99.50  99.67100.67  99.34  99.00Mean 
�RSD %    99.88 
    � 0.73100.14
 � 0.66   100.07
 � 0.91    99.99
  � 0.84 99.77
 � 1.19V0.370.770.930.951.36S.E0.230.410.580.671.16t-value b0.971.341.091.47F-value b2.112.672.433.11Tramadol ampoules2.5-100.25  99.50  99.67  99.25101.252.599.34100.67  99.50  99.00100.505.099.15  99.25101.00100.50  99.677.599.67  99.00  99.25  99.67  99.83Mean 
�RSD %99.60 
   � 0.6699.61
    � 0.8199.86
   � 0.7199.50 
 � 0.58100.31V0.310.890.350.27S.E0.220.700.210.16t-value b1.171.630.970.87F-value b2.473.372.122.04
a Average of six determinations.
b The theoretical values of t and F are 2.57 and 5.05, respectively at confidence limit at 95% confidence level and five degrees of freedom. 

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