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2022 ◽  
Vol 8 (4) ◽  
pp. 270-279
Anup K Chakraborty ◽  
Harshita Tripathi ◽  
Sarita Karole ◽  
Kavita R Loksh

is a significant therapeutic plant has a place with family apocynaceae contains in excess of 70 distinct sorts of chemotherapeutic agents and alkaloids which help in treating different illnesses. For the most part, it is known as Vincarosea, Ammocallisrosea and Lochnerarosea. There are numerous or more than 400 alkaloids present in plant, which are used as flavor, agrochemicals, pharmaceuticals, fragrance, ingredients, food addictives, and pesticides. To develop a validated high performance thin layer chromatographic method for the analysis of leaves and flower extracts of Sample solutions were applied onto the plates with automatic TLC sampler Linomat V (Camag, Muttenz, Switzerland) and were controlled by WinCATS software. Plates were developed in 10 x 10cm twin trough glass chamber (Camag, Muttenz, Switzerland). A CAMAG TLC scanner was used for scanning the TLC plates. Pre-coated silica gel aluminium plates 60F254. For vincristine, simultaneous estimation of vincristine was performed by HPTLC on a silica gel plate using toluene-methanol-diethylamine (8.75: 0.75: 0.5, v/v/v) as the mobile phase. The method was validated as per the ICH guidelines. The Rf value was found to be 0.76 for flower and 0.80 for leaves at 250 nm which shows the presence of vincristin in . In this research paper, a validated HPTLC Method has been developed for the analysis of leaves and flower extracts


Objective: The current study focused on the development, validation, and characterization of forced degradation products using LC-MS/MS. Methods: A simple, selective, validated and well-defined isocratic HPLC methodology for the quantitative determination of Tucatinib at a wavelength of 239 nm. An isocratic elution of samples was performed on an Inertsil ODS (250x4.6 mm, 5m) column with a mobile phase of 70:30v/v Acetonitrile and formic acid (0.1%) delivered at a flow rate of 1.0 ml/min. MS/MS was used to characterize degradation products formed in the forced degradation study. The validation and characterization of forced degradation products were performed in accordance with ICH guidelines. Results: Over the concentration range of 5-100μg/ml, a good linear response was obtained. Tucatinib's LOD and LOQ were determined to be 0.05 and 0.5, respectively. According to standard guidelines, the method was quantitatively evaluated in terms of system suitability, linearity, precision, accuracy, and robustness, and the results were found to be within acceptable limits. The drug was degraded under acidic, alkaline, and reduction conditions in forced degradation studies. Conclusion: The method was found to be applicable for routine tucatinib analysis. Because no LC-MS/MS method for estimating tucatinib and its degradation products has been reported in the literature. There is a need to develop a method for studying the entire tucatinib degradation pathway.

V. N. V. KISHORE ◽  

Objective: Stability representing the RP-HPLC method was established for synchronized quantification of Tigecycline and its impurities. This method was confirmed for its applicability to both tablet dosage and bulk drug forms. Methods: Intended for an isocratic elution, a mobile phase containing methanol: 10 mmol Triethylamine Buffer mixture (75:25 v/v, pH 6.1) was used at 1 ml/min flow rate and Agilent ZORBAX Eclipse XDB C18 (250 mm × 4.6 mm, 5 μm) column. Results: At 231 nm as wavelength, high-pitched peaks of Tigecycline (Tig) and its impurities (1and2) were detected at 6.55, 8.73 and 4.87 min correspondingly. The linearity of tigecycline and its impurities (impurity-1 and 2 and) were estimated with ranging from 75–450 µg/ml for Tigecycline and 1–6 µg/ml for both impurity 1 and 2. The corresponding recognition limits (LOD and LOQ) of the tigecycline and its impurities were originated to be (1.37,0.047 and 0.071 µg/ml) and (4.15, 0.143 and 0.126 µg/ml). Conclusion: The technique was effectively stretched for stability signifying studies under different stress conditions. Justification of the method was done as per the current ICH guidelines.


Objective: This method is focused on developing a precisely simplified and more accurate Reverse Phase–High Pressure Liquid Chromatography (RP-HPLC) method for the determination of Dapagliflozin in bulk and pharmaceutical dosage form as per guidelines of International Council for Harmonization (ICH). Methods: Evaluation and validation carried out using the RP-HPLC ZORBAX (C18) column (250 x 4.6 mm, 5 μm particle size) with a mobile phase consisting of Phosphate Buffer: Acetonitrile: Methanol in a ratio of 55:40:05 (v/v/v) at a flow rate of 1 ml/min with an injection volume of 10 μl. Results: Dapagliflozin was eluted at 2.12±0.05 min and detected at 225 nm. The regression equation y = 55762 x-29679 found to be linear with correlation coefficient r2 value of 0.9997. The developed RP-HPLC method was conveniently validated as per the ICH guidelines and found method was robust, sensitive, accurate, selective, specific, precise and linear. Conclusion: The proposed method was found to be accurate, precise, and robust for API and pharmaceutical dosage form as per experimentation analysis. The above developed method was found to be satisfied for Active Pharmaceutical Ingredient (API) and pharmaceutical formulation of Dapagliflozin to study its degradation products.


Objective: A novel, simple, precise, accurate, sensitive, and reproducible HPLC method for determining clopidogrel bisulfate in Wistar rat plasma was developed and validated. Methods: The chromatographic separation was performed using Xterra C18 (250 x 4.6 mm, 5μ) column. Mobile phase composed of Acetonitrile ACN: 0.05M potassium dihydrogen orthophosphate buffer pH 4.2 and in the ratio of 75:25% v/v at a flow rate of 1.2 ml/min. Detection was carried out using a PDA detector at 220 nm. The bioanalytical clopidogrel method was validated as per ICH guidelines. Results: The selected chromatographic condition was found to efficiently separate clopidogrel bisulfate (RT-2.838 min). The calibration curve was linear over the concentration range 40-200 ng/ml in Wistar rat plasma with a correlation coefficient of 0.999, respectively. The precision study revealed that the cumulative percentage variation was within the acceptable limit, and accuracy research showed the value of mean percent recovery between 99.72-99.83 %. Conclusion: A simple, rapid, specific, accurate, and precise analytical method was developed and validated using Wistar rat plasma. The technique was strictly validated according to the ICH guidelines. Acquired results demonstrate that the proposed strategy can be effortlessly and advantageously applied for routine analysis of clopidogrel in the Wistar rat plasma.

Pharmacia ◽  
2022 ◽  
Vol 69 (1) ◽  
pp. 45-50
Virab Gurgen Kirakosyan ◽  
Avetis Hovhannes Tsaturyan ◽  
Lilit Eduard Poghosyan ◽  
Ella Vardan Minasyan ◽  
Hayk Razmik Petrosyan ◽  

An isocratic, high-performance liquid chromatography (HPLC) quantitation method was developed for the quantitative determination of metformin, glibenclamide, gliclazide, glimepiride in some antidiabetic biologically active additives. A Nucleosil C18, 5 μm, 4.6 mm × 150 mm, column with mobile phase containing buffer (10 mm Na2HPO4, 10 mm sodium dodecyl sulfate): acetonitrile = 68 : 32 (V/V), pH = 7.5 was used. The flow rate was 1.0 mL/min, and effluents were monitored at 226 nm. The retention times of gliclazide glibenclamide, glimepiride and metformin, were 2.203, 4.587, 5.667 and 10.182 min, respectively. Linearity was studied by preparing standard solutions of gliclazide, glibenclamide, glimepiride and metformin at the concentration range of 50% to 150% of working concentration from a stock solution. The method was successfully applied to the estimation of gliclazide, glibenclamide, glimepiride and metformin in some antidiabetic biologically active additives. This method was validated to confirm its system suitability, selectivity, linearity, precision and accuracy according to international conference on harmonization (ICH) guidelines.

2022 ◽  
Vol 8 (1) ◽  
Challamalla Pavani ◽  
E. Susithra

Abstract Background The present research article involves the simultaneous determination of Tenofovir alafenamide, Darunavir, Emtricitabine and Cobicistat in bulk as well as in tablet dosage form using high performance liquid chromatography. Result The separation was performed using DIKMA Spursil, C18, ODS, (4.6 × 150 mm × 5 µm) analytical column using the mobile phase acetonitrile and 0.1% Orthophosphoric acid in the volume ratio of 70:30 at pH 3. The eluents were detected using PDA detector at 254.0 nm. After optimization subsequent validation study of different parameters was performed by utilizing the optimised condition as per the ICH guidelines. Under this optimised conditions Tenofovir alafenamide, Darunavir, Emtricitabine and Cobicistat were eluted at 2.287 min, 2.507 min, 4.062 min, 6.011 min respectively. Percentage assay was found 99.21% for Tenofovir alafenamide, 99.80% for Darunavir, 99.80% for Emtricitabine and 99.84% for Cobicistat. Tenofovir alafenamide was found linear in the range of 2.0–10.0 µg/mL, Darunavir (160.0–800.0 µg/mL), Emtricitabine (40.0–200.0 µg/mL) and for cobicistat (30.0–150.0 µg/mL). The corelation coefficient was found 0.999 for all the APIs. The detection limit was found 0.14 µg/mL for Tenofovir alafenamide, 2.14 µg/mL for Darunavir, 0.6 µg/mL for Emtricitabine and 7.32 µg/mL for cobicistat. In the LOQ study the quantitation limit was found 0.47 µg/mL for Tenofovir alafenamide, 7.12 µg/mL for Darunavir, 2.10 µg/mL, for Emtricitabine and 24.42 µg/mL for cobicistat. Conclusion All the studied API’s has been highly resolute utilizing the optimised condition and found extremely suitable for the determination of all of them simultaneously in marketed dosage form as well as in the bulk form.

2022 ◽  
pp. 47-74
Bhavna ◽  
Abhijeet Ojha ◽  
Samir Bhargava

2021 ◽  
Vol 12 (4) ◽  
pp. 368-376
Mahmoud Mohamed Abbas ◽  
Amira Mabrouk El-Kosasy ◽  
Lobna Abd El-Aziz Hussein ◽  
Nancy Magdy Hanna

Simple, accurate, and eco-friendly spectrophotometric procedures were proposed and implemented for simultaneous determination of anticoccidial drugs from three different classes namely, amprolium hydrochloride (AMP), sulfaquinoxaline sodium (SQX) and diaveridine hydrochloride (DVD). Dual wavelength in ratio spectra procedure was proposed where the difference in amplitudes (ΔP) in the ratio spectra at 264 nm and 301.9 nm (ΔP264&301.9 nm) corresponded to AMP with mean percentage recovery 100.00±0.923%, while (ΔP250.9&279 nm) and (ΔP218&243.5 nm) corresponded to SQX and DVD with mean percentage recoveries 99.31±1.083 and 100.64±1.219%, respectively. The dual wavelength in ratio spectra procedure was validated according to the ICH guidelines and accuracy, precision and repeatability were found to be within the acceptable limit. Multivariate chemometric approaches, namely, partial least-squares (PLS-2) and principal component regression (PCR) were also proposed with mean percentage recoveries 99.31±0.769, 98.91±1.192 and 99.04±1.245% for AMP, SQX and DVD, respectively, in PLS-2 and 99.63±1.005, 99.11±1.272 and 98.93±1.338% for AMP, SQX and DVD, respectively, in PCR. These procedures were successfully applied to the multi-ingredient veterinary formulation with mean percentage recoveries 100.75±1.238, 99.29±0.875 and 99.34±0.745% for AMP, SQX and DVD, respectively, in dual wavelength in ratio spectra procedure and 101.03±1.261, 101.48±0.984 and 101.10±1.339% for AMP, SQX and DVD, respectively, in PLS-2 and 100.22±1.204, 101.10±0.546 and 100.91±0.677% for AMP, SQX and DVD, respectively, in PCR.

2021 ◽  
Vol 4 (5) ◽  
pp. 01-08
Venkata Kishore ◽  
V. Tejeswara Rao ◽  
D. Aditya Deepthi ◽  
N. Annapurna

A novel, simple and economic high performance liquid chromatography (HPLC) method has been developed for the estimation of Clofarabine in bulk and tablet dosage form with greater precision and accuracy.The method was validated as per ICH guidelines. Validation studies demonstrated that the proposed HPLC method is simple, specific, rapid, reliable and reproducible. Hence the proposed method can be applied for the routine quality control analysis of Clofarabine in bulk and tablet dosage forms. All the components of the system are controlled using SCL-10Avp System Controller. Data acquisition was done using LC Solutions software.

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