Determination of Acceptable Residual Limit by Using Newly Developed and Validated RP-HPLC Method for Citalopram Hydrobromide Residues that Swabbed from Surfaces of Pharmaceutical Manufacturing Equipment

2019 ◽  
Vol 9 (01) ◽  
pp. 10-14
Author(s):  
Indu Bala ◽  
Surajpal Verma ◽  
Anzarul Haque ◽  
Bhupinder Singh
Keyword(s):  
Method Development ◽  
The United States ◽  
Hplc Method ◽  
Study Data ◽  
Assay Method ◽  
Manufacturing Equipment ◽  
Rp Hplc ◽  
United States Food ◽  
Development And Validation ◽  
Visual Limit

In this study, easy and robust RP-HPLC method was developed and validated to determine acceptable residual limit of citalopram hydrobromide for cleaning procedures. The United States, Food and Drug Administration has mentioned that the acceptable limit for residues present in the equipment during processing or manufacturing should be based on logical criteria. In present study, acceptable residual limit for cleaning procedure of citalopram hydrobromide was calculated by using three approaches including therapeutic dose method, 10 ppm criteria and visual limit of inspection. The value by erapeutic dose approach was less among three calculated values hence, selected as acceptable residual limit (10.66 µg/25 cm2 ) for analytical method development and validation for the detection of this drug residues on the surfaces of manufacturing equipment. A RP-HPLC assay method was developed using C18 column and mobile phase containing mixture of methanol and ammonium acetate buffer (pH4.6) (70:30) with flow rate of 1.6 ml/min. System suitability parameters like theoretical plates and tailing factor were calculated for the validation of the developed method as per ICH Q2B guidelines. After analyzing recovery study data, it was found that stainless steel plate has minimum recovery (88.87%) and pre-analyzed tablet solution has maximum recovery (99.29%)

scholarly journals RP-HPLC Method Development and Validation for Cleaning Residue Determination of Tofacitinib Citrate in Tofacitinib Tablets

2021 ◽  
pp. 262-276
Author(s):  
Thaticherla Kaleswararao ◽  
Duvvuri Suryakala
Keyword(s):  
Method Development ◽  
Drug Product ◽  
Hplc Method ◽  
Solution Stability ◽  
Sample Analysis ◽  
Validation Data ◽  
Manufacturing Equipment ◽  
Rp Hplc ◽  
Hplc Method Development ◽  
Development And Validation

A novel, Specific, and precise RP-HPLC method was developed to determine the residue content of Tofacitinib citrate left on the surface of equipment used in the manufacturing process. The manufacturing equipment considered in assessment of cleaning has been verified and found the tools assembled to the equipment are made up of Stainless steel, Glass, Teflon and plastic. Hence, these surfaces of manufacturing equipment that come in contact with the drug product during manufacturing are considered for evaluation of the cleaning procedure. By developing and validating an analytical method for residue estimation, the manufacturing equipment can be evaluated for efficient cleaning and to release the manufacturing equipment for further intended use by minimizing the cross contaminations. The stationary phase suited for the well separation of components is CAPCELL PAK C18 150 x 4.6 mm, 3 μm; 0.4 % perchloric acid and acetonitrile in the ratio of 85:15 % v/v is the mobile phase pumped at a flow rate of 1.2 mL/min through the column at temperature of 40 ºC. Each run extended for 10 min as the Tofacitinib peak elutes at RT of 5.2 min. The method has been validated successfully for Specificity, Precision, Linearity, Accuracy, Ruggedness and Filter validation of both rinse and swab methods. The LOD, LOQ concentrations found to be 0.006, 0.019 µg/mL for swab method and 0.03 and 0.1 µg/mL for rinse method respectively. The correlation coefficient is 0.999 and method found linear from LOQ to 500% for swab method and LOQ to 200% for rinse method. Solution stability has been established to ensure the test solution get tested within the stable time (4 Days). Based on the filter validation data, it is concluded that PVDF filter is not suitable for cleaning sample analysis and 2 mL sample should be discarded when 0.45 µm Nylon filter is used for cleaning sample analysis.

scholarly journals Stability Indicating RP-HPLC Method Development and Validation for Dexamethasone

2020 ◽  
Vol 32 (3) ◽  
pp. 587-591
Author(s):  
Pankaj N. Kulkarni ◽  
C.K. Jadhav ◽  
A.S. Nipate ◽  
Alaknanda M. Dodake-Supekar ◽  
C.H. Gill
Keyword(s):  
Method Development ◽  
Reversed Phase ◽  
Hplc Method ◽  
Assay Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Phase Water ◽  
Hplc Method Development ◽  
Development And Validation

A new, simple, reliable and reproducible stability indicating RP-HPLC assay method has been developed for quantitative analysis of dexamethasone from dexamethasone tablets. This developed method has been validated according to ICH guideline with respect to system suitability, specificity, precision, linearity, accuracy and robustness. An isocratic condition of mobile phase water (0.1% orthophosphoric acid):acetonitrile in a ratio of 60:40, v/v at a flow rate of 1.0 mL/minute over RP 2.5 Fortis C18, 100 × 4.6 mm, 2.5 μm, column was at 27 ºC maintained. This method is specific and showed excellent linear response with correlation coefficient (R2) values of 0.999. In forced degradation, the proposed method has been investigated with different stress conditions as hydrolytic, oxidative, thermal and humid as recommended by ICH guidelines. An accurate and reliable reversed-phase HPLC method for the analysis of dexamethasone in dexamethasone tablets was developed and validated successfully.

Stability Indicating Assay Method Development and Validation of Simultaneous Estimation of Chlorzoxazone, Diclofenac Sodium and Paracetamol in Bulk Drug and Tablet by RP-HPLC

2021 ◽  
pp. 5024-5028
Author(s):  
Krutika Patel ◽  
Sudheer Kumar Verriboina ◽  
S.G. Vasantharaju
Keyword(s):  
Method Development ◽  
Diclofenac Sodium ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Assay Method ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Bulk Drug

A simple, accurate, specific and stability-indicating RP-HPLC method was developed for simultaneous determination of chlorzoxazone, diclofenac sodium and paracetamol, using C18 Vydac Monomeric 120A (250 × 4.6mm, 5μ) at 40ºC. The mobile phase contains a mixture of 20mM potassium dihydrogen phosphate buffer (pH 6.2 adjusted with potassium hydroxide) and acetonitrile (30:70 v/v). The flow rate was 1ml/min and detection was carried out at 275nm using PDA detector. The retention time of paracetamol, chlorzoxazone and diclofenac sodium were 3.28mins, 13.27mins and 15.61mins respectively. The analytical curve was linear over a concentration range of 0.65- 6.5μg/ml for paracetamol, 1-10μg/ml for chlorzoxazone and 0.1-1μg/ml for diclofenac sodium. The drugs in bulk and tablet were subjected to acid and alkali hydrolysis, oxidation, thermal and photolytic degradation. This method can be successfully employed for simultaneous quantitative analysis of Chlorzoxazone, Diclofenac sodium and Paracetamol in bulk drug and tablet formulation.

scholarly journals RP-HPLC method development and validation for estimation of rivaroxaban in pharmaceutical dosage forms

2013 ◽  
Vol 49 (2) ◽  
pp. 359-366 ◽  
Author(s):  
Mustafa Çelebier ◽  
Tuba Reçber ◽  
Engin Koçak ◽  
Sacide Altinöz
Keyword(s):  
Method Development ◽  
Internal Standard ◽  
Hplc Method ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Hplc Method Development ◽  
Development And Validation ◽  
Tablet Dosage

Rivaroxaban, an anti-clotting medication, acts at a crucial point in the blood-clotting process and stops the formation of blood clots. In this study, RP-HPLC method was developed for the determination of rivaroxaban in tablets (Xarelto® (10 mg)). Phenomenex Luna 5 µm C18 100 Å LC Column (250 x 4.6 mm) was used at 40 ºC. Isocratic elution was performed with ACN:Water (55:45 v/v) mixture. The flow rate was 1.2 mL min-1 and UV detection was at 249 nm. Internal standard (Caffeine) and rivaroxaban were eluted within 2.21 and 3.37 minutes, respectively. The developed method was validated according to the ICH guidelines and found to be linear within the range 0.005 - 40.0 µg mL-1. The method was accurate, precise, robust and rapid. Thus, it was applied successfully for the quality control assay of rivaroxaban in tablet dosage form.

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