Pharmaceutical Analysis Articles

TROUBLESHOOTING IN HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

About Authors:
Ipshita Chattopadhyaya, Ekta Malhotra
Department of Pharmacy,
Jaipur National University,
Jaipur, India

ABSTRACT
(1)The developments in column packing technology and suitable equipment paved the way for what is now called High Performance or High Pressure Liquid Chromatography (HPLC). The new technique provided much higher resolution, more accurate quantitative results, as well as shorter analysis times in comparison to the earlier techniques .During the sixties, new theoretical insights accompanied by important. Since its introduction, HPLC has evolved into an indispensable tool in many analytical laboratories and is applied to diverse analytical problems. Actually, HPLC refers to a number of separation techniques that use a liquid mobile phase, or eluent. Troubleshooting HPLC instrumentation and separations require a fundamental understanding of how the instrument functions and how the separation works. (2)This article provides a practical guide to common HPLC problems, along with more in-depth information to help the reader understand the relationships between the observed symptoms and the underlying causes. The practical approach presented here is meant to serve as both a troubleshooting guide and an HPLC learning tool.

ESTIMATION OF SPIRONOLACTONE AND TORSEMIDE IN COMBINED TABLET DOSAGE FORM USING BY MULTICOMPONENT MODE OF ANALYSIS

About Authors:
Kapil Sharma1*, Subhash Gupta 2, Yogesh Sharma1
1 Yaresun Pharmaceuticals Pvt. Ltd.Jaipur - 302006, Rajasthan, India.
2 Oasis test house ltd.jaipur-302006,
Rajasthan, India.

SPECTROPHOTOMETRIC SIMULTANEOUS ESTIMATION OF SPIRONOLACTONE AND TORSEMIDE IN COMBINED TABLET DOSAGE FORM USING BY MULTICOMPONENT MODE OF ANALYSIS

ABSTRACT
A method for simultaneous estimation of torsemide (TRS) and spironolactone (SPL) in combined tablet dosage form has been developed. The method employs the application of multicomponent mode of analysis. This method utilize 50 % v/v methanol in distilled water. TRS show maximum absorbance at a wavelength of 288 nm and SPL at 238 nm. Where the linearity ranges for TRS and SPL were 1-5µg/ml and 5-25 µg/ml respectively. The procedure was successfully applied for the simultaneous determination of both drugs in laboratory prepared mixture and in market available tablet dosage form. The accuracy of the method was assessed by recovery studies and was found to be 98.15±0.64 and 100.27±0.15 for TRS and SPL respectively. Results of the analysis were validated statistically so that it can be used for routine analysis of TRS and SPL in combined tablet dosage form.

VALIDATION OF ANALYTICAL PROCEDURES: A COMPARISON OF ICH Vs PHARMACOPOEIA Vs FDA

About Authors:
Kataria Sahil,Middha Akanksha, Sandhu Premjeet
Seth G. L. Bihani S.D. College of Technical Education,
Institute of Pharmaceutical Sciences and Drug Research,
Sri Ganganagar, Rajasthan, INDIA

ABSTRACT
Method validation is the process used to confirm that the analytical procedure employed for a specific test is suitable for its intended use. Results from method validation can be used to judge the quality, reliability, and consistency of analytical results; it is an integral part of any good analytical practice. When extended to an analytical procedure, depending upon the application, it means that a method works reproducibly, when carried out by same or different persons, in same or different laboratories, using different  reagents,  different  equipment etc.  In  this  review  article  we  discussed  about  the  strategy  and  importance  of  validation  of  analytical  methods.

QSAR Analysis on Some Novel 4-Quinolylhydrazone Derivatives as Anti- Tubercular agent

About Authors:
Dr. A. K. Pathak, Parul Sengar, Kamlesh Kumar*
Department of Pharmacy, Barkatullah University
Bhopal, M. P.

Abstract
A Quantitative Structure Activity Relationship study on a Series of 40 molecules of (4-Quinolylhydrazone compounds) with anti-tubercular activity analogues was made using combination of various physicochemical descriptors (Thermodynamic, electronic and spatial). Several statistical expressions for 2D QSAR & 3D QSAR were developed using stepwise partial least square (PLS) regression analysis and K-Nearest neighboring molecular field analysis (K-NNMFA) respectively. The studies on 2D-QSAR, suggested the four descriptors T_C_C_2, T_C_N_4, Surface area excluding P & S, SsCH3E-index, and H donor count were common and highly contributed the activity. 2DQSAR model developed using partial least square regression approach. Negative logarithmic value of (MIC) was taken as dependent variable and selected discriptors were taken as independent varable. The analysis resulted in the following 2D-equation suggest that, MIC50 = [+0.1587 T_C_C_2- 0.0593 SsCH3E-index- 0.1395 T_C_N_4+ 0.3888 H-Donor Count -3.1556], n =26; Degree of freedom = 22; r2 = 0.75; q2 = 0.67; F test = 22.63;  r2 se = 0.20 ; q2 se = 0.23; pred_r2 = 0.46 ; pred_r2 se = 0.24, a H-donor group at Ar, is important for guiding the design of a new molecule. 3DQSAR model developed using K-nearest neighbour method (training set =33 and test set = 7). The best model derived by the method have q2 = 0.51, q2_se = 0.25, Predr2 = 0.71, pred_r2se = 0.16, n=33, k Nearest Neighbor is 2, Degree of freedom =28. The steric and electrostatic descriptors at the grid points, E_916 (0.1865, 0.3006); S_591 (-0.2851, -0.2580); S_1027 (-0.3273, -0.3090); S926 (30.000, 30.000) plays important role for design of new molecule. 3DQSAR analysis of series of 4-Quinolylhydrazone compounds informed that electropositive and less bulky group increases the biological activity.

Simultaneous Estimation of Aceclofenac and Paracetamol in Synthetic Mixture by Q-Analysis UV Spectrophotometric Method

About Author: Ashish Kumar Verma1, D.Raj. Anand1, Garima A. Tewari2
1.    Jubilant Chemsys Limited Noida 201301
2.    Babu Banarsi Das University Lucknow

ABSTRACT
Aceclofenac and paracetamol in combination are available as tablet dosage forms in the ratio of 1:5. A simple, reproducible and efficient method for the simultaneous determination of aceclofenac and paracetamol in synthetic mixture was developed. The proposed method is based on the Q-analysis UV Spectrophotometric method. The absorbance maxima of aceclofenac and paracetamol were found to be 275.4 nm and 248 nm, respectively in methanol. In Q-analysis, the isoabsorptive point for both the drugs was found at 266.1 nm. The linearity range lies between 1-35 µg/ml for aceclofenac and 1-15 µg/ml for paracetamol at their respective wavelengths. Both the drugs obey Beer’s law. The recovery studies confirmed the accuracy of the proposed methods.

METHOD DEVELOPMENT AND ITS VALIDATION FOR ESTIMATION OF TORSEMIDE IN TABLET DOSAGE FORM

About Authors:
Kapil Sharma1*, Subhash Gupta 2, Yogesh Sharma1
1 Yaresun Pharmaceuticals Pvt. Ltd.Jaipur - 302006, Rajasthan, India.
2 Oasis test house ltd.jaipur-302006,
Rajasthan, India.

METHOD DEVELOPMENT AND ITS VALIDATION FOR ESTIMATION OF TORSEMIDE IN TABLET DOSAGE FORM BY RP-HPLC AND UV SPECTROPHOTOMETRY AND COMPARISON OF TWO DEVELOPED METHODS BY USING t-TEST

ABSTRACT
One HPLC and one UV spectrophotometric method have been developed for the determination of torsemide (TRS) in tablet dosage form. The first method is based on determinetion of TRS in tablet dosage form by RP- HPLC method.  Chromatgraphy was carried out on a nucleosil C-18,250 x 4.6 mm column using a mixture of phosphate buffer and methanol  (50:50 v/v)  as the mobile phase at a flow rate of 1.3 ml/min.  Run time was 15 min.  Detection was done at 288 nm and retention time of the drug was 7.05 min.  This method produced linear responses in the concentration range 60-140  µg/ml of torsemide. The accuracy of the method was assessed by recovery studies and was found to be 99.90± 0.41 for torsemide.  The second method is based on the estimation of torsemide in tablet dosage form by UV spectrophotometry using 50% v/v methanol in distilled water.  Beer’s law obeyed over the concentration range 2-26 µg/ml at 288 nm with apparent molar absorptivity of 1.26 x 104.  Both developed methods were found to be applicable for routine analysis of drug in tablet dosage form. The result of the analysis were validated statistically.The results were compared obtained from UV spectrophotometry and HPLC.

QUANTITATIVE DERTERMINATION IN COMPARISION OF RAMIPRIL IN PURE FORM WITH OTHER PHARMACEUTICAL DOSAGE FORM BY USING RP – HPLC

About Authors:
Rajkumar Bolledula*, Priyanka.Mare1, Sunanda.Mare2
*Department of pharmaceutical analysis, Assistant professor in MITS college of pharmacy, H.No.41-64-s, saibabanagar, Kurnool-518004, A.P, India.
1.Department of pharmaceutics, Assistant professor, Mits college of pharmacy, Block .no.mc2/2, singareni colony, tekulapally,yellandu,khammam-507123,A.P,India
2.Department of pharmacology, J.K.K.Natarajan college of pharmacy, Salem, Tamil Nadu

ABSTRACT
This article describes the quantitative determination of percentage of drug concentration in pure and in formulated pharmaceutical dosage forms by using RP-HPLC. Procedure does not require prior separation of components from the sample.The mobile phase consists of methanol-water (80:20 v/v) for RP-HPLC with injection volume of 20μl.The RP-HPLC method was developed on a C-8 (150x4.6mm) column with detection carried out by variable wavelength detector at 209nm and 220 nm for ramipril, cardace, odopril respectively…Thus the Rt values obtained for different dosage forms are 1.59,1.44,1.34,1.35…..respectively with the concentration of 100% for pure drug and 97.54%,91.03%,65.76%.......respectively.

Development of HPTLC Finger Printing of Different Variety of Piper Betle Linn Leaf Oil Grown in Tamilnadu

About Author:
Sugumaran M., T. Vetrichelvan
Department of Pharmaceutical Chemistry,
Adhiparasakthi College of Pharmacy,
Melmaruvathur - 603 319, Tamilnadu , India

Abstract
High performance thin layer chromatographic finger print parameters had been developed for  Piper betle leaf oilisolated from karpoori, sirugamani and vellaikodi variety available in tamilnadu to fix standards. At shorter wavelength (254 nm) resolution was better for, so, this wavelength can be taken for obtaining optimum HPTLC finger printing for  volatile oil of this medicinal plant leaves. As per the data,   Karpoori variety of piper betle leaf oil  only showed  presence of  eugenol content. So, essential oil obtained from this variety should be included in the commercial tooth paste to get  antimicrobial activity against dental pathogens when compared to other studied variety.

METHOD DEVELOPMENT AND VALIDATION OF QUETIAPINE FUMARATE BY RP - HPLC METHOD

About Author:
Sharath Kumar Pallikonda*1, Srikanth Subburu2, Shanker Reddy Soma2, Chandra Shekar Reddy3
1,2Vathsalya College Of Pharmacy,
Bhongir, Dist: Andhra Pradesh, India - 508 116

Abstract
A simple, sensitive, rapid, robust and reproducible method for the determination of Quetiapine fumarate in bulk and pharmaceutical formulation (Tablets) was developed using reverse phase high performance liquid chromatographic method (RP-HPLC). The RP-HPLC analysis was performed isocratically on XTERRA C18 (4.6X150mm), analytical column using a mobile phase consisting of ortho phosphorus buffer and acetonitirle in the Ratio of 60:40v/v, with a flow rate of 0.6ml/min. The analyte was monitored with UV detector at 290nm. The developed method Quetiapine fumarate elutes at a run time of 10 min. The proposed method is having linearity in the concentration range from 40 to 80 μg/mL of Quetiapine fumarate. The present method was validated with respect to system suitability, linearity, precision, limit of detection (LOD) and limit of quantification (LOQ), accuracy (recovery), ruggedness, and robustness. The proposed method can be readily utilized for bulk drug and pharmaceutical formulations.

SIMULTANEOUS DETERMINATION AND VALIDATION OF TELMISARTAN AND RAMIPRIL IN PHARMACEUTICAL DOSAGE FORM BY RP – HPLC AND HPTLC

About Author:
B. Raj kumar*, M. Priyanka1, K. V. Subrahmanyam2, Syed Mujtaba Ahmed3, Ch. RakeshReddy1, R. Prem Sagar1

*Department of Pharmaceutical Analysis
Mits College of Pharmacy, kodad, Nalgonda

1. Department of Pharmaceutics
Mits College of Pharmacy, Kodad, Nalgonda
2. Department of Pharmaceutical Analysis
PIPS, Suryapet, Nalgonda
3. Department of Pharmaceutical chemistry
Netaji college of Pharmacy, Choutuppal, Nalgonda

Abstract:
The present work deals with the studies carried out on the development, optimization and validation of RP-HPLC and HPTLC methods for the simultaneous estimation of Telmisartan and Ramipril in combined dosage form. Market is folded with combination of drugs in various dosage forms. The multi-components formulations have gained a lot of importance now days due to greater patient acceptability, increased potency, multiple action, fewer side effects and quicker reliefs. For simultaneous estimation of drugs present in multi-component dosage form, High Pressure Liquid Chromatography (HPLC) and High Pressure Thin Layer Chromatography (HPTLC) methods are considered to be most suitable since it is extremely precise, accurate, sensitive, linear and rapid.  The literature survey carried out and it revealed that several analytical methods have been reported for estimation of these drugs as individual or in combination with other drugs. So the objective of the work is to develop HPLC and HPTLC methods for simultaneous estimation of drugs in multi-component dosage form for which no analytical method has been previously reported. Hence, present study have been planned to develop a specific, precise, accurate, linear, simple and rapid HPLC and HPTLC methods for simultaneous estimation of Telmisartan and Ramipril in tablet dosage form.

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