Eco - Friendly Method for the Estimation of Bisacodyl in Pharmaceutical Preparations and Environmental Wastewater Samples: Application to Content Uniformity Testing

Ahmed NR and Al-Etewi MJE

Published on: 2023-10-10

Abstract

 A simple, precise, accurate, rapid, economical and sensitive ultraviolet spectrophotometric method has been developed for the determination of Bisacodyl in pharmaceutical preparations and environmental wastewater samples, which shows maximum absorbance at 263 nm in ethanol (95%). Beer's law was obeyed in the range of 2.5-60μg/ ml, with molar absorptivity of 5. 3 ×103 L.mol-1.cm-1, relative standard deviation of the method was less than 1.8%, and accuracy (average recovery %) was 100 ± 1.0. The method was successfully applied to the determination of Bisacodyl in some pharmaceutical formulations (Tablets) and in environmental water samples. The proposed method was validated by sensitivity and precision which proves suitability for the routine analysis of Bisacodyl in true samples.

Keywords

Bisacodyl; Environmental Samples; Tablets; Uv spectrophotometry

Introduction

Bisacodyl (dulcolax); Figure (1) chemically is 4,4`(pyridin - 2 – yl methylene) bis(phenyl acetate) [ C22H19NO4 =361.4] is a laxative used for the treatment of constipation, for evacuation of the colon before radiological examination of the abdomen, or endoscopy, and before or after surgical operations. It has little or no action on the small intestine. Doses of 5 to 10 milligrams may be given by mouth and acute within 6 to 12 hours. Suppositories of 10 milligrams given by rectum act within one hour. Children under 10 years may be given 5 milligrams by mouth or by rectum [1-4].

4,4`-(Pyridin-2-ylmethylene)bis(phenyl acetate) C22H19NO4 361.4

Figure 1: Chemical Structure of Bisacodyl.

The literature survey reveals that) only few methods have been reported for determination of Bisacodyl in pure form and in pharmaceutiacal formulations [5-12]. Official method includes potantiometric titration for pure form and Uv spectrophotometric method for tablets and suppositories [5] .The spectrophotometric method include charge transfer and ion-pair complexion reaction [6] and indirect spectrophotometric method [7] .Other methods reported for determination of bisacodyl like stability-indicating methods [8], high-performance liquid chromatography [9], high performance thin-layer chromatography [10] , membrane sensor [11] and square-wave voltammetry [12] .The present work describes a new, simple indirect, spectrophotometric method for the determination of bisacodyl in pure form ,pharmaceutical formulations and in water samples. The method, which absorbs maximally at 263 nm.

Experimental

Apparatus

Shimadzu UV- 1700 pharmaspec (double beam) spectrophotometer with 1.0 cm quartz cells was used for absorption measurement.

Reagents

All chemical used were of analytical or pharmaceutical grade and Bisacodyj standard material was provided from AL-hokamaa company for pharmaceutical industries (HPI) Mosul-Iraq.

A standard solution 100ppm

This solution was prepared by dissolving 10 mg of Bisacodyl in 100 ml of ethanol 95% in calibrated flask.

Determination of Absorption Maxima

The standard solution of Bisacodyl (30µg/ml) was scanned in the range of 220-300nm which shows maxima located at 263 nm (Figure 2). Therefore, 263 nm wavelength was selected for the construction of calibration curve.

Figure 2: Absorption spectra of 30µg/ml Bisacodyl against ethanol (95%).

Recommended Procedure

From the absorption maxima, calibration curve was prepared in the concentration range of 2.5-60 µg/ml .The absorbance was measured at 263 nm against ethanol 95% as blank. The concentration of the sample solution can be determined by using the calibration curve.

Procedure for Pharmaceutical Preparations (Tablets)

Weight and powder 10 tablets. Dissolve a quantity of the powdered tablets containing 0.01 gm of Bisacodyl in about 100 ml ethanol and mixed for 20 mint and then filtered. The filtrate was mad up to 100 ml with ethanol and aliquot of this solution was treated as described above for recommended procedure and the concentration was calculated by using the calibration curve of this method. .

Procedure for real water samples: To demonstrate the practical applicability of the proposed method, real water samples were analyzed by this method. Industrial waste water from AL-hokamaa company for pharmaceutical industries (HPI) Mosul-Iraq, were fortified with the concentrations in the range of 5, 30, 50 µg/ml of Bisacodyl. The fortified water samples were analyzed as described above for recommended procedure and the concentration was calculated by using the calibration curve of this method.

Result and Discussion

UV? Visible spectrophotometry is still considered to be a convenient and low cost method for the determination of pharmaceuticals [13-15]. The method used for the determination of Bisacodyl in pharmaceutical preparations and environmental wastewater samples was found to be sensitive, simple, accurate, and reproducible .Beer s law was obeyed in the concentration range of 2-30 µg/ml (Figure 3) with correlation coefficient of 0.999, intercept of 0.0003 and slope of 0.014 .The conditional molar absorptivity was found to be 5. 3 x103 l/mol.cm.

Figure 3: Calibration curve for Bisacodyl.

The accuracy and precision of the method, a pure drug solution was analyzed at three different concentrations, each determination being repeated six times. The relative error (%) and relative standard deviation values are summarized in (Table 1).From (table 1) the values of standard deviation were satisfactory and the recovery studies were close to 100% . The RSD% value is less than 1.6 indicative of accuracy of the method.

Table 1: Accuracy and precision of the proposed method.

Bisacodyl taken

( µg/ml)

Er (%)a

RSD (%)

2

15

30

2.15

15.21

30.16

1.6

1.55

1.5

a: Mean of six determinations.

Analytical Application

The proposed method was satisfactorily applied to the determination of Bisacodyl in its pharmaceutical preparations tablets and wastewater samples, the results of the assay of the pharmaceutical preparations revels that there is close agreement between the results obtained by the proposed method and the label claim (Table 2), and the results of water samples (Table 3) show that the recovery values obtained were closed to 100%.

Table 2: Determination of Bisacodyl formulations.

Pharmaceutical formulations

Proposed method found*

Label amount

Bisacodyl (HPI)

5. 2 mg/tablet

5mg/tablet

Bisacodyl (NDI)

3.05 mg/tablet

3mg/tablet

*Mean of five determinations

Table 3: Determination of Bisacodyl in industrial wastewater samples.

Wastewater samples

Added µg/ml

Found* µg/ml

Recovery % (n=10)

Industrial wastewater

5

5.02

100. 4

30

30.06

100.2

50

50. 06

100. 12

* Mean value of ten determinations.

Application of the Proposed Method to Content Uniformity [16-18]

Content uniformity or the Uniformity of dosage unit was defined as the degree of uniformity in the amount of active substance among dosage units. The risk assessment strategy underlying content uniformity testing is the assumption that some pre-specified limits exist where safety and efficacy outcomes may change if content uniformity fails. The proposed method proved to be suitable for the content uniformity test, where a great number of assays on individual tablets are required. Data presented in table 4 indicate that the proposed method cans accurately and precisely quantitative losartan potassium in its commercially available tablets. The mean percentage (with RSD) of the labeled claim found in ten tablets was 100.06 (0.3132%) which fall within the content uniformity limits specified by the United State Pharmacopeia [17].

Table 4: Content uniformity testing of tablets using the proposed method.

Parameter

% of the label claim

Table No.1

100. 1

Table No.2

99. 9

Table No.3

100.4

Table No.4

100.3

 Table No.5

99. 8

Table No.6

100.1

Table No.7

99.8

Table No.8

100.2

Table No.9

100,2

Table N0.10

99.8

Mean(X)

100.06

%RSD

0.32

Max. allowed unit value[17]

±15%

Conclusion

The developed method is found to be sensitive, accurate, simple, precise and economical, and can be used for routine quality control analysis of Bisacodyl in pure form, bulk, pharmaceutical formulations and environmental wastewater samples.

Acknowledgments

The authors wishes to express gratitude to AL-hokamaa company for pharmaceutical industries (HPI) Mosul-Iraq, for providing gift samples of Bisacodyl standard materials and tablets.

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