Pharmaceutical Analysis Articles

About Authors:
Bhawana Kapoor^*1, Vishnukant Rai², Sonu Sharma^3
1Seth G.L. Bihani S.D. College of Technical Education, Sriganganagar, Rajasthan, India
²Shri Ramnath Singh College of Pharmacy, Gormi, Bhind, M.P., India
³NIMS Institute of Pharmacy, Jaipur, Rajasthan, India

ABSTRACT
Chromatography, although primarily a separation technique, is mostly employed in chemical analysis in which High-performance liquid chromatography (HPLC) is an extremely versatile technique where analytes are separated by passage through a column packed with micrometer-sized particles. Now a day reversed-phase chromatography is the most commonly used separation technique in HPLC. The reasons for this include the simplicity, versatility, and scope of the reversed-phase method as it is able to handle compounds of a diverse polarity and molecular mass. This review covers the importance of RP-HPLC in analytical method development and their strategies along with brief knowledge of critical chromatographic parameters need to be optimized for an efficient method development.

About Authors:
Ujjwal S. Yeotkar*, Mahendra Nimbhorkar, Tushar A. Deshmukh, Vijay R. Patil
Department of Pharmacognosy,
Tapi Valley Education Society’s,
Hon’ble, Loksevak Madhukarrao Chaudhari College of Pharmacy,
North Maharashtra University,
Faizpur- 425 503,
Maharashtra, India.

ABSTRACT
Churna are important group of formulation used by Ayurvedic physicians to treat various types of diasease. Trikatu and Pimpali churna, as per Ayurvedic literature is used for the treatment of resperatory disorders. In the present study,an attempt has been made to develop a HPTLC  method of quantitative estimation of marker compound, piperine in laboratory prepared authentic formulation and a marketed formulation of Trikatu and Pimpali churna. The stationary phase used was precoated silica gel G ₆₀ F ₂₅₄ plates. The mobile phase containing n- Hexane-ethyl acetate, (5:5 v/v ), was used to separate the spot of Piperine. Plates were developed to a distance of 8 cm at room temperature. Spectrodensitometric scanning was performed by TLC scanner III (CAMAG) in absorbance mode at the wavelength of 339nm. The  R_f  values of  piperine was 0.44± 0.02. The method was validated in terms of Linearity, Accuracy and  Precision. The linearity curve found to be linear in between 200–900 ng/spot. The limit of Detection (LOD) and limit of Quantification (LOQ) were found to be  1 ng and  3 ng respectively. The mean results from % Recovery was found to be, laboratory formulation contain 85.13% and 83.47% while the commercial formulation shows 96.65%, and 90.32% respectively. The proposed method can be used to determine Piperine from Ayurvedic formulations.

About Authors:
Snehal V.Chopade, Dr.V.R.Patil - Principle
TVES College of pharmacy,
Faizpur accredited by North Maharashtra University,
Jalgaon

Abstract:
UPLC can be regarded as new invention for liquid chromatography. UPLC refers to Ultra Performance Liquid Chromatography. UPLC brings dramatic improvements in sensitivity, resolution and speed of analysis can be calculated. It has instrumentation that operates at high pressure than that used in HPLC & in this system uses fine particles(less than 2.5µm) & mobile phases at high linear velocities decreases the length of column, reduces solvent consumtion & saves time.
This review introduces the theory of UPLC, and it can summarizes some of the most recent work in the field.

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.

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.

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.

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.

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.

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.