RP-HPLC Method Development and Validation for Simultaneous Estimation of Mirabegron and Silodosin in Synthetic Mixture

 

Ashvin V. Dudhrejiya1, Shivangi B. Pithadiya1,2*, Amitkumar J. Vyas1, Nilesh K. Patel1,

Ajay I. Patel1, Hetal B. Gavit3, Dhruvanshi A. Gol1

1B. K. Mody Government Pharmacy College, Rajkot, India.

2Department of Pharmaceutical Science, Faculty of Health Sciences, Marwadi University,

Gujarat, 360003, India.

3Government Pharmacy Collage, Surat, India.

*Corresponding Author E-mail: shivangipithadiya1999@gmail.com

 

ABSTRACT:

Background: The primary objective of the present study of RP-HPLC technique by utilizing a UV detector that possesses characteristics of simplicity, sensitivity, speed, accuracy, and precision. The present study employed a methodology to concurrently determine the quantities of Mirabegron and silodosin within a synthetic blend. Material and Method: RP-HPLC Method was developed by using isocratic elution mode. Using an OROSIL C18 column that measured 150mm in length, 4.6mm in Column inside Diameter (ID), and 3µm in particle size, the materials were separated by liquid chromatography. The mobile phase employed was a blend of methanol and phosphate buffer at a 60:40% v/v ratio. And 0.5ml/min wasflowing rate, the separation was accomplished. Using a UV detector, all of the compounds were identified and measured at a wavelength of 270nm. Result: For Mirabegron and Silodosin, the linearity of the technique was seen within the range of concentration for 6.3-150 ppmand 2-48µg/ml, respectively. The range of percentage recovery for Silodosin was 98.05% to 100.23%, and for Mirabegron it was 98.86% to 100.64%. The methodology was verified in compliance with the International Council on Harmonization's criteria (Q2R1). Conclusion: The suggested RP-HPLC technique is highly appropriate for analyzing Mirabegron and Silodosin, as it guarantees precise findings without any interference.

 

KEYWORDS: Mirabegron, Silodoisn, HPLC, Synthetic Mixture, Validation.

 

 

INTRODUCTION: 

Mirabegron (MIRA) is a compound with the chemical formulaC₂₁H₂₄N₄O₂S.1 Mirabegron has complex structure, which is made up of Thiazole ring, Acetophenone moiety and benzyl group. Silodosin also referred to as SILO, is identified by Molecular Formula C25H32F3N3O4. Chemical structure of silodosin is characterized by Thieno[2,3-d]pyrimidin-4-ylamine core and it is attached with 2-[(2R)-2,3-Dihydro-1-(2-hydroxyethyl)-2-oxo-1H-inden-5-yl]acetamide2. By specifically activating the β3-adrenoceptors on the bladder's detrusor muscle, mirabegron helps the bladder fill and store urine without interfering with the contractions that cause the bladder to void.

 

The alpha (α)-1A subtype has the highest affinity for silodosin, which specifically inhibits alpha(α)-1A adrenergic receptors. These two drugs are combined to treat both benign prostatic hyperplasia (BPH) and overactive bladder (OAB).3-5

 

This fixed-dose combination is being studied in a clinical trial phase three. The dosage ratio of MIRA and SILO in this bilayer tablet is 3.2:1.6 In BPH complicated with OAB people, coadministration of MIRA and SILO was well tolerated with no notable adverse events. Figure 1 displays the SILO and MIRAc hemical structures.

 

(a)

 

(b)

Figure 1: Chemical structure of (a) Mirabegron and (b) Silodosin.

 

According to the literature review, SILO is recognized by JP, while MIRA is not recognized by any pharmacopoeia7. Several analytical techniques for measuring MIRA and SILO both by itself and in mixed with other drugs were published, including UV spectroscopy8–11, HPLC12–14, RP-HPLC15–42, UPLC43, HPTLC44–45, LC/MS-MS46, UHPLC47, and LC-ESI-MS/MS48. Therefore, it makes sense to develop a method that can be used with a combination of predetermined doses that is scientific, sensitive, and well-developed. The created approach can be used for regular analysis in research labs or the pharmaceutical industry.

 

MATERIALS AND METHODS:

Software, Materials and Reagents:

Thermo - HPLC was utilised and results were analyzed with chromeleon software. MIRA came from CTX Life Science, and SILO from Prudence Life Science. Using lactose, magnesium stearate, sorbitol, and microcrystalline cellulose as the excipients, the synthetic mixture was prepared. and HPLC-grade methanol, acetonitrile, water, and AR-grade phosphate buffer as the mobile phase.

 

Procedure for Determining the Sampling Wavelength:

To determine the wavelength at which both medications show maximum absorption, methanol (200–400nm) was used as a blank and mirabegron (25ppm) and silodosin (8ppm) were scanned independently. The wavelength of 270nm was chosen for silodosin and mirabegron based on their overlapping spectra. The Spectrum is illustrated in Figure 2.

 

 

Figure 2 : Determination of Maximum Wavelength

 

Chromatographic Condition:

Thermo HPLC was utilized, and Cromeleon software was used to process the data. Using an isocratic elution mode and an OROSIL C18(150mm, 4.6mm, 3µm) column, chromatographic separation was carried out. MeOH and phosphate buffer (pH:4.0) (60:40% v/v) make up the mobile phase. A 2µl injection volume was employed, with a 0.5ml/min flow rate at 270nm.

 

Preparation of Standard Stock Solution:

50mg of MIRA and 16mg of SILO were added to a VF with a 100ml capacity using an exact weight measurement. MIRA and SILO were found to be 500 ppm and 160ppm, respectively, after around 50ml of methanol was added and ultrasonically dissolved to the necessary level.

 

Preparation of Synthetic Mixture:

The medication MIRA (50mg) and SILO (16mg) were added to a 100ml volumetric flask together with common tablet excipients (lactose, mannitol, magnesium stearate, and microcrystalline cellulose) as gliding, diluent, dissolving, and binder, respectively. After adding around 50ml of methanol and sonicating it until it totally dissolved, the concentration was increased to 500ppm for MIRA and 160ppm for SILO. Once 10 milliliters of the appropriate solution are pipetted out as needed, dilute with methanol to get the final concentrations of 32μg/ml for SILO and 100μg/ml for MIRA.

 

System Suitability Parameter:

The chromatographic system's suitability was evaluated by six replicate injections.

 

Method Validation:49

Linearity:

A standard stock solution was, subsequently, diluted with MeOH to produce a concentration in series of 6.3- 150ppm of MIRA and 2- 48ppm of SILO, respectively.

 

Accuracy:

Drug-to-drug spiking was performed to test accuracy at three unique analyte concentrations: 50%, 100%, and 150%. Concisely, a drug recovery study was performed by spiking of 25µg/ml, 50µg/ml, 75µg/ml of MIRA, and 8µg/ml, 16µg/ml, 24µg/ml of SILO to the produced mixture containing 50µg/ml of MIRA and 16µg/ml of SILO.comprising 16µg of SILO and 50µg of MIRA per milliliter.

 

Precision:

Six duplicates were utilised to assess the repeatability of the 50ppm MIRA and 16ppm SILO doses. The three concentration levels of 50%, 100%, and 150% were reached in triplicate for the intraday and interday fluctuations of both drugs (25, 50, and 75ppm for MIRA and 8, 16, and 24ppm for SILO).

 

Limit of Quantification (LOQ) and Limit of Detection (LOD):

To determine the method's sensitivity, LOD and LOQ were calculated..

 

Specificity:

The test for excipient interference, specificity was assessed using six duplicates at doses of 50ppm of MIRA and 16ppm of SILO, both with and without the excipients added. The % interference was used to determine the method's specificity.

 

Robustness:

A minor deliberate modification in the method parameters, such as the flow rate difference by ±0.05 ml/min, the mobile phase ratio variation by ±1.0ml organic solvent, and the temperature fluctuation by ±1.0 ○C, was utilised to find the method’s robustness.

 

RESULTS AND DISCUSSION:

Optimize Chromatographic Condition:

The ideal mobile phase composition in isocratic elution mode was MeOH: Phosphate buffer (60:40% v/v) (pH:4.0) with an OROSIL C18(150mm, 4.6mm, 3µm) column. UV detection was carried out at a wavelength of 270nm, with a flow rate of 0.5ml/min established. The mobile phase was filtered and degassed prior to use.with a 0.2µm membrane filter made of nylon. The chromatogram of the ideal condition is shown in Figure 3, and the system suitability parameters are expressed in Table 1.

 

 

Figure 3: Chromatogram of optimizing condition

 

Table 1: System suitability parameter

Sr. No

Name

Retention time ±SD

Area±SD (µAU)

Asymmetry ±SD

Resolution ±SD

Theoretical plate ± SD

1

MIRA

3.953±0.1

188071.82 ± 5000.24

1.41 ± 0.1

1.28 ±

2514 ± 100

2

SILO

5.808 ± 0.1

54380.29 ±1000.20

1.28 ± 0.1

-

7015 ± 120

 

     

(A)                                                                                                                       (B)

Figure 4: linearity of (A)Mirabegron, (B)linearity of Silodosin

 

Analytical Method Validation:48

Linearity:

SILO and MIRA had linearity ranges of 2–48ppm and 6.3–150µg/ml, respectively, according to reports. It was discovered that the correlation coefficients for SILO and MIRA were, respectively, 0.9994 and 0.9993. The curves representing linearity are presented in Figures 4 (A) and (B).

 

Specificity:

% interference was computed, and the result was less than 0.5%. As a result, the approach is particular.

 

Accuracy:

The percentage recovery for SILO and MIRA ranged from 98.05 to 100% and 98.86 to 100%, respectively. As a result, Table 2 presents result for an accuracy study and the percentage of medicines retrieved is sufficient.

 

Table 2: Recovery data of mirabegron and silodosin analyzed by the developed RP-HPLC method.

% Recovery level

AssayConc.(µg/ml)

Spiked Conc.(µg/ml)

% drug Recoveryrange(n=3)

MIRA

SILO

MIRA

SILO

MIRA

SILO

50

50

16

25

8

99.07-99.13

98.41-98.42

100

50

16

50

16

99.58-99.86

98.05-99.02

150

50

16

75

24

100.18-100.64

100.23-100.87

 

Table 3: Repeatability study data Mirabegron and silodosin.

Drug

Concentration (µg/ml)(n=6)

Area (µg/ml)Mean ± SD

RSD

MIRA

50

211554.52 ± 41.74

0.0001

SILO

16

60869.77 ± 405.38

0.006

 

Table 4: Intraday and interday precisions of Mirabegron and silodosin.

Precision

 

Interday (n=3)

Intraday (n=3)

DRUG

Level (%)

Area (Mean ± SD) (µAU)

RSD

Area (Mean ± SD) (µAU)

RSD

MIRA

50

106966.21±3.78

0.003

107967.94±2.51

0.0023

100

211572.34±2.99

0.0014

205965.43 ±57.23

0.027

150

330505.11±4.94

0.0014

318015.02 ±5.56

0.0017

SILO

50

30506.47 ± 5.75

0.01

30444.82 ±5.09

0.016

100

58630.83± 5.65

0.009

60704.06 ±8.34

0.01

150

91053.82 ± 5.46

0.005

94930.005 ± 8.70

0.009

 

Precision:

RSD was found <2 will show adequate precision of the method. results for both are given in Tables 3 and 4.

 

LOD and LOQ:

For MIRA and SILO, the corresponding LOD and LOQ were found to be 1.34ppm and 4.08ppm and 0.07ppm and 0.22µg/ml.

 

Robustness:

This study demonstrated that the process stayed the same with just deliberate variations. The suggested approach is robust, as indicated by the determined RSD of less than two.

 

Assay:

After calculating the % assay for the synthetic mixture, the outcome was judged satisfactory. The result is expressed in Table 5.

 

Table 5: Result of assay of the synthetic mixture

Name of Drug

Label claim (mg)

Amount found (mg)

% Assay (n=6) ± SD

MIRA

25

25.45

101.8 ± 0.2

SILO

8

7.95

99.4 ± 0.2

 

CONCLUSION:

MIRA and SILO in a synthetic combination can be measured simultaneously using an easy-to-use, low-cost RP-HPLC technique. For MIRA and SILO, the linearity was found to be 6.3-550g/ml and 2-48g/ml, respectively. An RSD of less than 1 was obtained from the precision and repeatability analysis, and the percentage recovery for MIRA and SILO was found to be between 98.86 and -100.64% and 98.05 and -100.23%, respectively. This means that there should be no issues when using this method to examine dose forms. It is quick, simple to grasp, precise, inexpensive, reliable, and accurate.

 

ACKNOWLEDGEMENT:

B. K. Mody Government Pharmacy College in Rajkot has provided The facilities to perform this experiment. Gift samples of mirabegron and silodosin were provided by Prudance Pharmachem and CTX Life Sciences Pvt. Ltd.

 

REFERENCE:

1.      Sankar PR, et al. Analytical Method Development and Validation for The Determination of Mirabegron in Pharmaceutical Dosage Form By RP-HPLC. International Journal of Pharmaceutical Sciences and Research. 2020; 11(5): 2223-2228. doi: 10.13040/IJPSR.0975-8232.11(5).2223-28

2.      Sarika S. Malode, Milind P. Wagh. Formulation and Evaluation of Orodispersible Tablets Containing Taste Masked Mirabegron Resinate. Research Journal of Pharmacy and Technology. 2020; 14(9): 4736-2. doi: 10.52711/0974-360X.2021.00824.

3.      Rajendra K. Surawase, Kamalkishor G. Baheti. Box Behnken Design for Optimization of Mirabegron Solid Dispersion by Fluidized Bed Processing. Research Journal of Pharmacy and Technology. 2022; 15(4): 1472-6. doi: 10.52711/0974-360X.2022.00244

4.      Bhamre P, Rajput SJ. Spectrofluorimetric Method For the Determination of Silodosin In Bulk And Pharmaceutical Dosage Form. Indo American Journal of Pharmaceutical Research, 4(10): 5106-5110.

5.      Yoshihisa M, Shun T, et al. Comparison in the efficacy of fesoterodine or mirabegron add-on therapy to silodosin for patients with benign prostatic hyperplasia complicated by overactive bladder: A randomized, prospective trial using urodynamic studies. Wileyonlinelibrary. 2019; 33(3): 941-949. doi: 10.1002/nau.23935

6.      CDSCO-Drug combination approval, August 2021, https://cdsco.gov.in/opencms/opencms/en/Approval_new/CT-Approvals/

7.      Japanese Pharmacopoeia, 8th Edn, The ministry of Health, Labourand Welfare, 2017, 1573.

8.      Badike KS, Nerusula A, Anne BS. Analytical method development and validation for the estimation of mirabegron in pure and its solid dosage form by UV- spectrophotometric method. International Journal of Research in Pharmaceutical sciences and Technology. 2020; 1(4): 146-150. doi: https://doi.org/10.33974/ijrpst.v1i4.207

9.      Panchumarthy R, et al. Validated UV spectrophotometric method for quantitative determination of Mirabegron in bulk and Pharmaceutical dosage form. Der Pharmacia Lettre. 2016; 8(14): 96-103.

10.   Aneesh TP, Rajasekaran A. Method Development And Validation For The Estimation Of Sildosin In Bulk And Pharmaceutical Dosage Forms Using Uv-vis Spectrophotometry. Asian Journal of Pharmaceutical and Clinical Research. 2012; Aug 31; 5(4): 150-2.

11.   Pithadiya SB, Vyas AJ. Spectroscopic method development and validation of drug used In treatment of benign prostatic hyperplasia complicated with over active bladder. Journal of Medicinal and Nanomaterials Chemistry. 2024; 6(2): 116-125. doi: 10.48309/JMNC.2024.2.3 .

12.   Fan Z, Yuxia Z, et al. Liquid Chromatographic Separation and Thermodynamic Investigation of Mirabegron Enantiomers on a Chiralpak AY-H Column. Journal of Chromatographic Science. 2015; 53: 1361–1365. doi: 10.1093/chromsci/bmv025

13.   Engin Er, Nevin ErK. An effective and sensitive stability indicating chromatographic approach based on HPLC for silodosin assay. Journal of Analytical Science and Technology, 2016; 20(7): doi: 10.1186/s40543-016-0100-y.

14.   Aneesh TP, Rajasekaran A. Development And Validation Of Hplc Method For The Estimation Of Silodosin In Bulk And Pharmaceutical Dosage Form. International Journal of Biological & Pharmaceutical Research. 2012; 5(4): 693-696.

15.   Spandana R, Rao RN, et al. Analytical Method Development And Validation For The Estimation Of Mirabegron In Bulk And Pharmaceutical Dosage Form By RP-HPLC. Indo American Journal of Pharmaceutical Research. 2016; 11(5): 2223-2228.

16.   Jyothsna M, RayeesAhmed MD, et al. Method Development and Validation of Mirabegron in Bulk Drug and Pharmaceutical Dosage Form. Journal of Pharmacy and Biological Sciences. 2018; 13(1): 78-83. doi: 10.9790/3008-1301037883

17.   Suryawanshi R, Shaikh S, Patil S. RP-HPLC Method Development and Validation for the Estimation of Mirabegron in Bulk and Dosage Form. Journal of Drug Delivery & Therapeutics. 2020; 10(1): 31-38. Doi: https://doi.org/10.22270/jddt.v10i1.3829

18.   Rezari M, Ramazani A. RP-HPLC Method Development and Validation for the Quantitative Estimation of Mirabegron in Extended-Release Tablets. Journal of Medicinal and Chemical Sciences, 2018; 4(4): 308-410. doi: https://doi.org/10.26655/jmchemsci.2018.9.5

19.   Pigili R. Development and Validation of RPHPLC Method For Estimation of Silodosin In Bulk And Pharmaceutical Dosage Forms. International Journal of Pharmaceutical Science Review and Research. 2012; 16(2): 52-55.

20.   Harischandran S, et al. Validated Stability Indicating RP-HPLC Method for the Determination of Silodosin in Pharmaceutical Dosage Form. International Journal for Pharmaceutical Research Scholars. 2012; 1(4):141-145.

21.   Goud VM, et al. Method Development and Validation of RP-HPLC Method for assay of Sildosin in Pharmaceutical Dosage Form. International Journal of Pharma Sciences. 2013; 3: 194-196.

22.   Gupta A, Mishra SK. A Novel Analytical Method for Simultaneous Quantification of Silodosin and Tadalafil by RPHPLC. Journal of Pharmaceutical Research International. 2021; 33(39B): 194-202. https://doi.org/10.9734/jpri/2021/v33i39B32195

23.   Nataraj KS, et al. Analytical Method Development and Validation for the Estimation of Silodosin and Dutasteride in Capsule Dosage Form by RP-HPLC Method. Journal of Drug Metabolism & Toxicology. 2020; 11(2): 1-8. doi:10.35248/2157-7609.20.11.245

24.   Paljashuva K, Ramarao N. Simultaneous Estimation Of Dutasteride And Silodosin In Bulk Form By Rp-hplc Method. World Journal of Current Medical and Pharmaceutical Research. 2019; oct 31; 1(5): 148-163.

25.   Murugan S, Upendra Janardhan CH, Niranjan Babu M. RP-HPLC Method for Simultaneous Estimation of Albendazole and Niclosamide in Oral Suspension for Veterinary Use. Research J. Pharm. and Tech. 2016; 9(1): 27-32. doi: DOI: 10.5958/0974-360X.2016.00006.8

26.   V. Agrahari, M. Bajpai, S. Nanda. Essential Concepts of Mobile Phase Selection for Reversed Phase HPLC. Research J. Pharm. and Tech. 2013; 6(5): 459-464.

27.   Peethala Prathyusha, Raja Sundararajan, Palyam Bhanu, Mathrusri Annapurna Mukthinuthalapati. A new stability indicating RP-HPLC method for determination of Bilastine in bulk and pharmaceutical formulation. Research J. Pharm. and Tech. 2020; 13(6): 2849-2853. doi: 10.5958/0974-360X.2020.00507.7

28.   Merugu Manasa, Vijey Aanandhi M. Stability Indicating Method Development and Validation of Semaglutide by RP-HPLC in Pharmaceutical substance and Pharmaceutical Product. Research J. Pharm. and Tech. 2021; 14(3): 1385-1389. doi: 10.5958/0974-360X.2021.00247.X

29.   Baokar Shrikrishna, Ranpise Nisharani. Analytical Method Development and Validation for Simultaneous Estimation of Montelukast and Ebastine by HPLC. Research J. Pharm. and Tech. 2015; 8(1): 1-5. doi: 10.5958/0974-360X.2015.00001.3

30.   Sridevi. S, Vijayakumar. R, C. N. Nalini. Method Development and Validation for the Simultaneous Estimation of Ascorbic acid, Phenylephrine HCl, Paracetamol and Levocetirizine HCl using RP-HPLC. Research J. Pharm. and Tech. 2020; 13(4): 1911-1916. doi: 10.5958/0974-360X.2020.00344.3

31.   Vijaykumar T. Pawar, Shubhangi V. Pawar, Harinath N. More, Anita S. Kulkarni, Dinanath T. Gaikwad. RP-HPLC Method for Simultaneous Estimation of Cilnidipine and Chlorthalidone. Research J. Pharm. and Tech. 2017; 10(11): 3990-3996. doi: 10.5958/0974-360X.2017.00724.7

32.   Sapna MR, Paresh UP. Development and Validation of RP – HPLC Method for Estimation of Lamivudine and Dolutegravir Sodium in Synthetic Mixture. Research J. Pharm. and Tech. 2019; 13(6): 2864-2868. doi: 10.5958/0974-360X.2020.00510.7

33.   Thangabalan B, Salomi M, Sunitha N, Manohar Babu S. Development of validated RP-HPLC method for the estimation of Itraconazole in pure and pharmaceutical dosage form. Asian J. Pharm. Ana. 2013; 3(4): 119-123.

34.   Revathi R., Saravanan V.S., Ethiraj T., Jhansi Lakshmi Marreddy. RP-HPLC Analysis for Quantitation of Candesartan Cilexetil in Solid Dosage Forms. Asian J. Pharm. Ana. 2013; 3(4): 115-118.

35.   Sunitha N, Sindhura L, Thangabalan B, Manohar Babu S. Development and Validation of RP–HPLC Method for Simultaneous Estimation of Cefepime and Tazobactam in Injection Formulation. Asian J. Pharm. Ana. 2013; 3(4): 131-137.

36.   Vanaja N, Preethi Ch, Manjunath SY, Krishanu Pal. Method Development and Validation for Simultaneous Estimation of Telmisartan and Chlorthalidone by RP-HPLC in Pharmaceutical Dosage Form. Asian J. Pharm. Ana. 2015; 5(4): 171-177.

37.   Pawar J, Sonawane S, Chhajed S, Sanjay K. Development and Validation of RP-HPLC method for simultaneous Estimation of Metformin HCl and Gliclazide. Asian J. Pharm. Ana. 2016; 6(3): 151-154.

38.   Khan H, Ali M, Ahuja A, Ali J. Validated HPLC-UV Method for Simultaneous Determination of Some Anti-Inflammatory and Analgesic Drugs. Asian J. Pharm. Ana. 2016; 6(3): 183-187.

39.   Chandana OSS, Ravichandra Babu R. Stability Indicating High Performance Liquid Chromatographic Assay for the Determination of Sildenafil Tartrate. Asian J. Pharm. Ana. 2017; 7(3): 196-200.

40.   Wagh K, Sonawane S, Chhajad S, Kshirsagar S. Development of a RP-HPLC method for separation of ezetimibe in presence of atorvastatin caclium and simvastatin and its application for qunatitation of tablet dosage forms. Asian J. Pharm. Ana. 2017; 7(3): 169-175.

41.   Parmar A, Sonawane S, Chhajed S, Kshirsagar S. Development and validation of RP-HPLC method for simultaneous estimation of ezetimibe and glimepiride in tablet dosage form. Asian J. Pharm. Ana. 2017; 7(3): 185-188.

42.   Venkateswara Rao B, Vijetha P, Vidyadhara S, Kavitha K. A Novel RP-HPLC Method Development and Validation for the Determination of Pioglitazone and Glimepiride in Bulk and Pharmaceutical Formulations. Asian J. Pharm. Ana. 2017; 7(3): 145-150.

43.   Lanka RA, et al. New Rapid UPLC Method For The Estimation Of Impurities In The Capsule Dosage Form Of Silodosin. International Journal of Analytical and Bioanalytical Chemistry. 2012

44.   Sayana PS, et al. Development and Validation of HPTLC Method for Quantification of Silodosin in Bulk and Pharmaceutical Dosage Form. The Pharma Innovation. 2012; 1(10).

45.   Shah DA, et al. High-Performance Thin-Layer Chromatographic Method for the Estimation of Mirabegron and Solifenacin Succinate Used in the Treatment of Overactive Bladder Syndrome. Journal of planar chromatography- modern TLC. 2019; 32(4): 323-327. doi: https://doi.org/10.1556/1006.2019.32.4.7

46.   Parsha S, Ravindrakumar Y, Ravichander M. LC–MS/MS and NMR Characterization of Forced Degradation Products of Mirabegron. Journal of Liquid Chromatography & Related Technologies. 2016; 39(4): 178-194. doi: https://doi.org/10.1080/10826076.2016.1144201

47.   Jafer VS, Saladi S, Sait SS. Development of Stability-Indicating UHPLC Method for the Quantitative Determination of Silodosin and Its Related Substances. Journal of Chromatographic Science. 2013: 1-8. doi:10.1093/chromsci/bmt094

48.   Chiguru V, et al. LC-ESI-MS/MS evaluation of forced degradation behaviour of silodosin: in vitro anti-cancer activity evaluation of silodosin and major degradation products. Journal of Pharmaceutical and Biomedical Analysis. 2017; 134: 1. doi: 10.1016/j.jpba.2016.11.013

49.   ICH Harmonized Tripartite Guidelines (2005). Q2 (R1) Validation of Analytical Procedures: Text and Methodology.

 

 

 

Received on 18.05.2023            Modified on 11.01.2024

Accepted on 29.06.2024           © RJPT All right reserved

Research J. Pharm. and Tech 2024; 17(9):4247-4252.

DOI: 10.52711/0974-360X.2024.00656