scholarly journals Chaotropic effect of trifluoroacetic and perchloric acid on B-cyclodextrin inclusion complexation process with risperidone, olanzapine and their selected impurities

2020 ◽  
Vol 70 (6) ◽  
pp. 360-376
Author(s):  
Nevena Đajić ◽  
Jovana Krmar ◽  
Anđelija Malenović ◽  
Biljana Otašević ◽  
Ana Protić
Keyword(s):  
Trifluoroacetic Acid ◽  
Mobile Phase ◽  
Method Development ◽  
Desirability Function ◽  
Chaotropic Agent ◽  
Optimal Separation ◽  
Derringer’S Desirability Function ◽  
Complexation Process ◽  
Chaotropic Agents ◽  
Separation Conditions

Effective method development together with method`s eco-friendly character are gaining importance in drug analyses nowadays. One of the strategies often applied to improve the efficacy of separation methods, especially in the case of basic ionizable analytes is adding chaotropic salts into the mobile phases. Moreover, the development of the green liquid chromatography method could also be achieved with certain mobile phase additives such as cyclodextrin (CD). The study aims to investigate whether adding chaotropic agents could improve the complexation process by disrupting the analytes' water solvation shell. The model mixture consisted of risperidone, olanzapine, and their related impurities. Method development was aided with experimental design methodology, while optimal separation conditions were selected using Derringer's desirability function. Mathematical models obtained for each of the examined responses enabled the explanation of the single and simultaneous influence of b-CD concentration, chaotropic agents type, and content, as well as the content of acetonitrile in the mobile phase. Retention factors appeared to be the most influenced by acetonitrile content in the mobile phase. The type of chaotropic agent as well as its concentration lead to retention prolongation, but if acetonitrile content in the mobile phase is high, the effect of chaotropic agent becomes negligible. Interaction between analyte and b-CD are relatively weak in comparison to the interaction of analyte form with either chaotropic agent or acetonitrile. Interaction leading to complexation are outperformed by other analyte related interactions in this complicated system, so complexation based retention reduction is not fully exposed. However, increasing b-CD concentration shows a positive effect on the resolution between critical peak pairs. Optimal separation conditions were selected based on 3D plots of Derringer's desirability function. For olanzapine and its impurity, they included the following: acetonitrile content 16% (v/v), trifluoroacetic acid as a chaotropic agent with 0.95% (v/v) content, and 9 mM b-CD concentration. Further, optimal separation conditions for risperidone and its impurity were 25% (v/v) acetonitrile content in the mobile phase, trifluoroacetic acid as chaotrope agent with 0.27% (v/v) content and 5mM b-CD concentration.

A new metric for relating macroscopic chromatograms to microscopic surface dynamics: the Distribution Function Ratio (DFR)

The Analyst ◽  
2021 ◽  
Author(s):  
Logan Daniel Cruckson Bishop ◽  
Anastasiia Misiura ◽  
Christy F. Landes
Keyword(s):  
Distribution Function ◽  
Stationary Phase ◽  
Mobile Phase ◽  
Separation Efficiency ◽  
Surface Dynamics ◽  
Model Free ◽  
Optimal Separation ◽  
Phase Chemistry ◽  
Separation Conditions ◽  
Microscopic Surface

Heterogeneous stationary phase chemistry causes chromatographic tailing that lowers separation efficiency and complicates optimizing mobile phase conditions. Model-free metrics are attractive for assessing optimal separation conditions due to the low...

FORCED INDICATING UPLC-DAD METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF APALUTAMIDE IN BULK AND IN PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (09) ◽  
pp. 73-75
Author(s):  
China Babu D ◽  
Madhusudhana Chetty C ◽  
Mastanamma S. K ◽  
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Uv Light ◽  
Accurate Method ◽  
Pharmaceutical Dosage Form ◽  
Good Ability ◽  
Acquity Uplc ◽  
Development And Validation

A new analytical method was developed for the estimation of apalutamide in bulk and its pharmaceutical formulation. The sensitive, précise and accurate method was developed by using Waters Acquity UPLC system equipped with quaternary gradient pump. The column used was Waters C18 150 X 2.1 mm X 1.7 µm and mobile phase was 0.2 % OPA buffer in water : acetonitrile in the ratio of 25:75 V/V. The buffer pH was maintained at 4.5. The fl ow rate of mobile phase was 0.5 mL min-1 and detection was at 272 nm by using PDA detector. The method was performed at ambient temperature. The retention time of the apalutamide was 1.27 min. The % RSD value in precision was >2 %. The accuracy of the method was found to be between 99.54 % - 100.01 %. The limit of detection and limit of quantifi cation values were found to be 0.14 µg mL-1 and 0.48 µg mL-1, respectively. The linearity concentration range was found to be 11.25 - 67.5 µg mL-1, it show wide linearity concentration range. The method was proved to have good robustness after changing parameters of fl ow rate, temperature and mobile phase composition. The method showed good ability towards different stress conditions of acidity, alkalinity, peroxide and UV-light. The method can be used for the routine analysis of apalutamide in bulk and its pharmaceutical dosage form by using UPLC.

RP-HPLC METHOD DEVELOPMENT FOR THE ASSAY OF AMPHOTERICIN B

INDIAN DRUGS ◽  
2014 ◽  
Vol 51 (02) ◽  
pp. 16-20
Author(s):  
L Mohankrishna ◽  
◽  
P. J. Reddy ◽  
B. P Reddy. ◽  
P. Navya
Keyword(s):  
Amphotericin B ◽  
Mobile Phase ◽  
Method Development ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Phase Combination ◽  
Hplc Method Development

A sensitive and precise HPLC procedure has been developed for the assay of amphotericin B in bulk samples and pharmaceutical formulations by using a C18 column [Kromosil, C18, (5 µm, 4.6mm x 250 mm; Make. Waters)], and mobile phase combination is 1% formic acid in water and acetonitrile in ratio of 45:55 V/V. The procedure has been validated as per the ICH guidelines. The λmax of detection was fixed at 407 nm, so that there was less interference from mobile phase with highest sensitivity according to UV analysis. Calibration plots were linear in the range of 10-100 µg/mL and the LOD and LOQ were 0.02 µg/mL and 0.06 µg/mL respectively. The high recovery and low relative standard deviation confirm the suitability of the method for routine quality control determination of amphotericin B in different formulations.

scholarly journals RAPID ANALYTICAL METHOD FOR ASSAY DETERMINATION FOR PROCHLORPERAZINE EDISYLATE DRUG SUBSTANCES BY ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY

2017 ◽  
Vol 9 (4) ◽  
pp. 118 ◽  
Author(s):  
Kishorkumar L. Mule
Keyword(s):  
Liquid Chromatography ◽  
Trifluoroacetic Acid ◽  
Analytical Method ◽  
Mobile Phase ◽  
Ultra Performance Liquid Chromatography ◽  
Drug Substance ◽  
Assay Method ◽  
Column Temperature ◽  
Drug Substances

Objective: To develop and validate new, simple and rapid assay method for Prochlorperazine edisylate drug substance by UPLC as per ICH guidelines.Methods: Ultra performance liquid chromatographic method was developed, optimized and validated on Acquity UPLC by using Acquity BDH300 C4 (100 x 2.1 mm) 1.7µ column. 3.85g ammonium acetate in 1000 ml of water add 0.5 ml trifluoroacetic acid and 1 ml triethylamine (Mobile phase A): 0.5 ml trifluoroacetic acid in 1000 ml acetonitrile mobile phase (Mobile phase B) with gradient program. Detector wavelength 254 nm and column temperature 30 °C.Results: Linearity study was carried out for prochlorperazine edisylate, linearity was calculated from 80 % level to 120% with respect to specification level. The correlation coefficient (r) = 0.999 was proved that the method is robust. The resolution between known impurities and Prochlorperazine edisylate found more than 2.5, it was evident from specificity test that Prochlorperazine edisylate peak are well separated from its related impurities, hence the method is specific. Prochlorperazine edisylate sample solution and mobile phase were found to be stable for at least 3 d.Conclusion: A new, simple and rapid method has been developed and validated for assay determination of prochlorperazine edisylate in drug substance by Ultra Performance Liquid Chromatography (UPLC). The analytical method was developed and validated as per ICH guidelines. The developed method can be used for the fast assay determination of prochlorperazine edisylate drug substances in research laboratories and in the pharmaceutical industry. 

scholarly journals Pengaruh Substitusi Tepung Terigu dengan Tepung Umbi Dahlia dan Konsentrasi Baking Powder terhadap Karakteristik Fisik Cookies Kaya Serat

2020 ◽  
Vol 9 (4) ◽  
pp. 175-180
Author(s):  
Ahmad Zaki Mubarok ◽  
Ardelia Winata
Keyword(s):  
Physical Properties ◽  
Wheat Flour ◽  
Desirability Function ◽  
High Fiber ◽  
Powder Concentration ◽  
Wide Range ◽  
Powder Addition ◽  
Derringer’S Desirability Function ◽  
Optimum Formula ◽  
And Control

Cookies merupakan salah satu makanan ringan yang disukai disemua kalangan umur. Umumnya cookies terbuat dari tepung terigu, memiliki kandungan karbohidrat dan lemak yang tinggi namun mengandung kadar serat yang rendah. Pada penelitian ini tepung umbi dahlia digunakan sebagai substitusi tepung terigu untuk pembuatan cookies kaya serat. Tujuan dari penelitian ini adalah untuk mengkaji penggunaan tepung umbi dahlia sebagai substitusi tepung terigu dan konsentrasi baking powder dalam formulasi pembuatan cookies. Rasio tepung umbi dahlia dan tepung terigu pada penelitian ini yaitu 15:85, 30:70, dan 45:55; dan konsentrasi baking powder yang digunakan yaitu 1–3% dari berat tepung. Metode Derringer’s Desirability Function digunakan untuk mendapatkan formula terbaik, dengan membandingkan kedekatan nilai karakteristik fisik cookies yang diberi perlakuan dengan karakteristik fisik cookies kontrol sebagai target. Hasil penelitian ini didapatkan formula terbaik untuk pembuatan cookies kaya serat adalah penggunaan rasio tepung umbi dahlia dan tepung terigu sebesar 30:70 dan penggunaan baking powder konsentrasi 3% dengan nilai total desirability (D) sebesar 0,87. Kesimpulan dari penelitian ini adalah cookies kaya serat berhasil dapat diproduksi dengan menggunakan tepung umbi dahlia dan jumlah penambahannya yang terbaik, dapat ditentukan.Effect of Substitution of Wheat Flour with Dahlia Tuber Flour and Concentration of Baking Powder on Physical Properties of Fiber Rich CookiesAbstractCookies are one of the snacks favored by wide range of consumers’s age. Usually, cookies made from wheat flour, which have high content of carbohydrate and fat but low content of fiber. In the present study, dahlia tuber flour was used to substitute wheat flour to produce fiber rich cookies. The effect of dahlia tuber flour was analyzed in the a varied baking powder addition. Dahlia tuber flour and wheat flour at ratio of 15:85, 30:70, and 45:55 (w/w); and baking powder concentration of 1–3% from total weight of the flour was usedas formula. Optimum formulation was obtained by Derringer’s Desirability Function, which compares the relation value of the physical properties of cookies made with dahlia tuber flour and control cookies which was made of wheat flour. The result showed that optimum formula to produce fiber rich cookies was obtained on the ratio of 30:70 and baking powder at concentration of 3%, with total desirability (D) value of 0.87. As conslusion, high fiber content cookies was succsessfully produced and the best dahlia tuber flour addition was determined optimally.

scholarly journals KARAKTERISTIK FISIK COOKIES PADA BERBAGAI RASIO TERIGU DENGAN TEPUNG UMBI DAHLIA DAN PENAMBAHAN MARGARIN [Physical Properties of Cookies Made from Different Ratio of Wheat with Dahlia Tuber Flours and Addition of Margarine]

2020 ◽  
Vol 25 (2) ◽  
pp. 90
Author(s):  
Ahmad Zaki Mubarok ◽  
Solisa Vania Joelita Sembiring
Keyword(s):  
Physical Properties ◽  
Wheat Flour ◽  
Desirability Function ◽  
High Carbohydrate ◽  
Optimum Formulation ◽  
Derringer’S Desirability Function ◽  
D Value

Cookies are one of the snacks, usually made from wheat flour and have high carbohydrate and fat but low fiber contents. In the present study, dahlia tuber flour was used to substitute wheat flour to produce fiber-rich cookies. The effect of dahlia tuber flour and wheat flour ratio and the addition of margarine were studied. The optimum formulation was obtained by Derringer’s desirability function, by comparing the closeness value of the physical properties of cookies made from dahlia tuber flour with control cookies made from wheat flour as a target. The result showed that optimum formulation to produce fiber-rich cookies obtained by using dahlia tuber flour and wheat flour ratio of 30:70 and margarine 75%, with total desirability (D) value of 0.84.

ANALYTICAL METHOD DEVELOPMENT AND ITS VALIDATION FOR EVALUATION OF POLYHERBAL FORMULATION

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (10) ◽  
pp. 66-68
Author(s):  
◽  
A. P Jadhav
Keyword(s):  
Immune Response ◽  
Ethyl Acetate ◽  
Analytical Method ◽  
Mobile Phase ◽  
Method Development ◽  
Simultaneous Estimation ◽  
Active Constituents ◽  
Polyherbal Formulation ◽  
Marker Compounds ◽  
Hptlc Method

Talekt capsule is a branded polyherbal formulation used for enhancing the immune response to dermal infections and also for treating skin disorders. Curcumin and embelin, which are the active constituents of Haridra and Vidanga, respectively were used as marker compounds for developing a simple, accurate, precise and robust HPTLC method for simultaneous estimation. The mobile phase of toluene: ethyl acetate: formic acid (6.5: 3: 0.2 v/v/v) was used for separation. 381nm was used as wavelength for analysis. The Rf value obtained for curcumin, and embelin was found to be 0.51 ± 0.2 and 0.33 ± 0.2, respectively. The developed method was validated on the basis of ICH Q2 (R1) guidelines.

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