Journal of Synthetic and Natural Chemistry

B.J.M. Reddy et al.

J Syn Natu Chem, 2018;3(1):31-34 World Inventia Publishers

Journal of Synthetic and Natural Chemistry http://www.worldinventiapublishers.com/JSNC/ Vol. 3, Issue 1, 2018 Research Article A NEW RP-HPLC METHOD FOR THE SIMULTANEOUS ESTIMATION OF MAGALDRATE AND SIMETHICONE IN BULK AND TABLET DOSAGE FORM AS PER ICH GUIDELINES B. Madhavi Latha 1 *, MD. Noorjahan 1, Dr. A. Madhukar 2 * 1 Department of Pharmacy, Brilliant Grammar School Educational Society, Group of Institutions Integrated Campus (Faculty of Engineering & Faculty of Faculty), Abdullapurmet, Hyderabad, Telangana, INDIA. 2 Associate Professor, Avanthi Institute of Pharmaceutical Sciences, Gunthapally, R.R. Dist., Hyderabad, Telangana, INDIA.

Received on: 18-02-2018; Revised and Accepted on: 21-03-2018

ABSTRACT

A rapid and precise Reverse Phase High Performance Liquid Chromatographic method has been developed for the validated of Magaldrate and Simethicone, in its pure form as well as in tablet dosage form. Chromatography was carried out on a Hypersil C18 (4.6 x 150mm, 5µm) column using a mixture of Methanol: Water (80:20v/v) as the mobile phase at a flow rate of 1.0 ml/min, the detection was carried out at 310 nm. The retention time of the Magaldrate and Simethicone was 3.031 & 4.075 mints respectively. The method produce linear responses in the concentration range of 1050µg/ml of Magaldrate and 5-25µg/ml of Simethicone. The method precision for the determination of assay was below 2.0%RSD. The method is useful in the quality control of bulk and pharmaceutical formulations. KEYWORDS: Magaldrate, Simethicone, RP-HPLC, Validation. INTRODUCTION

Magaldrate is a common antacid drug that is used for the treatment of duodenal and gastric ulcers, esophagitis from gastroesophageal reflux. Magaldrate is chemically named as Hydroxymagnesium aluminate complex that is converted rapidly in gastric acid to Mg(OH)2 and Al(OH)3, which are absorbed poorly and thus provide a sustained antacid effect [1]. Simeticone (or simethicone in the USA) is an anti-foaming agent used to reduce bloating, discomfort or pain caused by excessive gas. Simeticone is used to relieve the symptoms of excessive gas in the gastrointestinal tract, namely bloating, burping, and flatulence [2]. There is a lack of evidence that simeticone is effective for this use [3, 4].

Fig. 2: Chemical Structure of Simethicone In the scientific literature, analysis of Magaldrate and Simethicone has been reported as individual ingredients and in combination with other compounds [5, 6]. No other chromatographic methods are found for simultaneous analysis of Magaldrate and Simethicone in a combined dosage form. The method described is rapid, economical, precise, and accurate and can be used for routine analysis of tablets. It was validated as per ICH guidelines [7-9]. MATERIALS AND METHODS

Fig. 1: Chemical Structure of Magaldrate

*Corresponding author:

B. Madhavi Latha Department of Pharmacy, Brilliant Grammar School Educational Society, Group of Institutions Integrated Campus (Faculty of Engineering & Faculty of Faculty), Abdullapurmet, Hyderabad, Telangana, INDIA. * E-Mail: [email protected]

Experimental: Materials: Pharmaceutical grade working standards Magaldrate and Simethicone were obtained from Hetero Labs, Jedcharla, India. All chemicals and reagents were HPLC grade and were purchased from Merck Chemicals, Mumbai, India. Instrumentation: The analysis was performed using Waters-2695 (Modal Alliance) High Performance liquid chromatography, analytical balance (Mettler Toledo), PDA Detector (Standard cell) and data handling system (Empower 2), pH meter (lab India), Sonicator. The column used is Hypersil C18 (4.6 x 150mm, 5µm) with the flow rate 1.0ml/min (isocratic).

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B.J.M. Reddy et al.

J Syn Natu Chem, 2018;3(1):31-34

Preparation of Mobile Phase: Accurately measured 800ml (80%) of Methanol and 200ml of Water (20%) a were mixed and degassed in digital ultrasonicater for 10 minutes and then filtered through 0.45 µ filter under vacuum filtration. Preparation of standard solution: Accurately weigh and transfer 10 mg of Magaldrate and Simethicone working standard into a 10ml of clean dry volumetric flasks add about 7ml of Methanol and sonicate to dissolve and removal of air completely and make volume up to the mark with the same Methanol. Further pipette 0.3ml of the Magaldrate (30 µg/ml) and 0.15ml of the Simethicone (15 µg/ml) from above stock solutions into a 10ml volumetric flask and dilute up to the mark with Methanol. RESULTS AND DISCUSSION

consists of 800ml (80%) of Methanol and 200ml of Water (20%). Then finally filtered using 0.45µ membrane filter paper and degassed in sonicator for 15 minutes. The detection is carried out using PDA detector at 310 nm. The solutions are following at the constant flow rate of 1.0 ml/min. The retention time for Magaldrate and Simethicone was 3.031 & 4.075 min respectively. Linearity ranges for Magaldrate and Simethicone were 10 - 50 μg/mL and 5 - 25 μg/mL respectively and the results were found in the acceptable as (R2) = 0.9994 & 0.9995 for Magaldrate and Simethicone respectively. LOD were 1.7µg/ml and 0.85µg/ml and LOQ were 5.6 µg/ml and 2.8μg/mL for Magaldrate and Simethicone respectively. The all parameters value of RSD is less than 2.0% indicating the accuracy and precision of the method. The percentage recoveries were found 100 - 101% and 99.0 - 100% for Magaldrate and Simethicone respectively.

The simultaneous estimation of Magaldrate and Simethicone was done by RP-HPLC and in the optimized method the mobile phase Table No. 1: Optimized Chromatographic Conditions Parameters Stationary phase (column) Mobile Phase Flow rate (ml/min) Run time (minutes) Column temperature (°C) Volume of injection loop (l) Detection wavelength (nm) Drugs RT (min)

Method Hypersil C18 (4.6 x 150mm, 5µm) 80:20v/v, (Methanol : Water) 1.0 8.0 35 10 310 3.031 & 4.075

Fig. 3: Optimized Chromatogram of Magaldrate and Simethicone at 310 nm Table No. 2: Linearity Data of Magaldrate and Simethicone Analyte Magaldrate Simethicone

Concentration range (μg/mL) 10 – 50 5 - 25

Correlation Coefficient (R2) 0.9994 0.9995

Slope

Intercept

29458x 17764x

10129 1368.9



B.J.M. Reddy et al.

J Syn Natu Chem, 2018;3(1):31-34

Fig. 4: Linearity Curve of Standard Magaldrate

Fig. 5: Linearity Curve of Standard Simethicone

Table No. 3: Repeatability and Reproducibility results of Magaldrate and Simethicone No. of Preparation Pre-1 Pre-2 Pre-3 Pre-4 Pre-5 Mean St. dev. % RSD

Repeatability 918705 910361 912476 910894 917558 913998.8 3873.258 0.423

Magaldrate Reproducibility 898219 898032 898132 898014 898044 898182.5 243.4829 0.027

Simethicone Repeatability Reproducibility 177255 122555 177532 122076 177993 122547 177433 122067 174028 122079 176848.2 122301.8 1599.934 250.7145 0.904 0.204

Table No. 4: System suitability parameters for Magaldrate and Simethicone System suitability parameters Retention time (min) %RSD for Repeatability of peak area Resolution (Rs) Tailing factor (asymmetric factor) USP plate count LOD (μg/mL) LOQ (μg/mL)

Magaldrate 3.031 0.423 1.09 2947 1.7 5.6

Simethicone 4.075 0.904 5.16 1.21 8872 0.85 2.8

Table No. 5: Robustness study for analytical method validation of Magaldrate and Simethicone

Magaldrate

Parameters Flow Rate ±0.1ml/min Mobile Phase (80:20) (±5ml)

Simethicone

Flow Rate ±0.1ml/min Mobile Phase (80:20) (±5ml)

a=

Adjusted to 0.9 ml/min 1.1ml/min 85:15 75:25 0.9 ml/min 1.1ml/min 85:15 75:25

Mean Area a 699451 718432 695471 695412 126954 129542 131654 128256

Mean RT 3.215 2.894 2.954 3.185 4.197 3.825 3.932 4.152

% RSD 0.29 0.71 0.64 0.27 0.19 0.68 0.34 0.81

5 Replicates

Tablet No. 6: Accuracy Results of Magaldrate and Simethicone Drug Name Magaldrate

Simethicone

%Concentration (at specification Level) 50% 100% 150% 50% 100% 150%

Area 453153 910568.3 1351727 134989.7 265939 401572.3

Amount Added (ppm) 15 30 45 7.5 15 22.5

Amount Found (ppm) 15.0 30.5 45.5 7.5 14.8 22.5



% Recovery 100% 101% 101% 100% 99% 100%

Mean Recovery 100.0%

99.6%

B.J.M. Reddy et al.

J Syn Natu Chem, 2018;3(1):31-34 CONCLUSION

5.

A new RP-HPLC method described in this manuscript provides a simple, convenient and reproducible approach for the simultaneous estimation and quantification of Magaldrate and Simethicone in routine quality control analysis.

6.

REFERENCES: 1. 2. 3. 4.

Laurence L, Brunton. Goodman & Gilman's The Pharmacological Basis of Therapeutics, 12th ed. "Simethicone tablet". NIH Daily Med. April 2016. Retrieved 27 August 2017. Modi Ronak, Clearfield Harris R, Levitt Michael. Belching, Bloating, and Flatulence. Am College of Gastroenterol 2013. Simethicone.drugs.com. Efficacy not established for the symptomatic relief of immediate postprandial upper abdominal distress.

7. 8. 9.

Satyanarayana et al. Method Development and Validation for Simultaneous estimation of Ranitidine, Domperidone and Simethicone in bulk and Pharmaceutical dosage form by using RP-HPLC Method. World J Pharm and Pharm Sci 2015;4(11):1146-1158. Firdous Hassanuddin, G. VIjaya Kumar, MA. Haneef. Validated High Performance Liquid Chromatography Method for Simultaneous Estimation of Magaldrate and Simethicone in API and Tablet Dosage form and its Application to Forced Degradation Studies. Int J Pharm Rev & Res 2018;8(1):12-18. Code Q2(R1)-Text on Validation of Analytical Procedure Step-3 Consensus Guideline. ICH Harmonised Tripartite Guideline, 2005. Code Q2A-Text on Validation of Analytical Procedure Step-3 Consensus Guideline. ICH Harmonised Tripartite Guideline, 1994. Code Q2B-Validation of Analytical Procedure Methodology Step4 Consensus Guideline. ICH Harmonised Tripartite Guideline, 1994.

How to cite this article: B. Madhavi Latha et al. A NEW RP-HPLC METHOD FOR THE SIMULTANEOUS ESTIMATION OF MAGALDRATE AND SIMETHICONE IN BULK AND TABLET DOSAGE FORM AS PER ICH GUIDELINES. J Syn Natu Chem 2018;3(1):31-34.

Conflict of interest: The authors have declared that no conflict of interest exists.

Source of support: Nil

