Pharmaceutical Analysis Articles

About Authors:
CHIRAG S. RAJPARA*¹, JAWED AKHTAR¹, AMIT KHANDHAR²
1. Department of Quality Assurance, School of Pharmaceutical Sciences, Jaipur National University, Jagatpura, Jaipur-302025, Rajasthan, India.
2. Zydus cadila pharma, moraiya,ahmedabad.
*chiragrajpara2601@gmail.com

ABSTRACT
* A simple, specific, accurate and stability-indicating reversed phase high performance liquid chromatographic method was developed for simultaneous estimation of Tadalafil and Dapoxetine HCL, Water Symmetry C-18 (150 x 4.6 mm),5 µ and a mobile phase composed of Buffer : Acetonitrile (65:35)

* The retention time of Tadalafil and Dapoxetine HCL were found to be10.08 and 4.45 min respectively. Linearity was established for Tadalafil and Dapoxetine HCL in the range of 8.0-60 μg/ml and 24.0-180.0 μg/ml respectively. The percentage recovery of Tadalafil and Dapoxetine HCL were found to be in the range of 99.7-100.6% and 98.07-99.09% respectively. The drug was subjected to acid and alkali hydrolysis, oxidation, dry heat and photolytic degradation. The degradation studies indicated, Tadalafil showed degradation in acid and alkali while it was found stable in H₂O_2, photolytic and in presence of dry heat and Dapoxetine showed degradation in thermal and peroxide while it was found stable in rest of parameters . The degradation products of Tadalafil and Dapoxetine HCL in acidic, alkaline conditions were well resolved from the pure drug with significant differences in their retention time values. This method can be successfully employed for the quantitative analysis of Tadalafil and Dapoxetine HCL in bulk drugs and formulations.

About Author:
Hardik Patel^*, Sagar Solanki
Department of Pharmaceutical Chemistry,
K.B.Raval College of Pharmacy, Shertha,
Gandhinagar-382423, Gujarat, India.
*patel1928@yahoo.in

ABSTRACT
A new, simple, rapid, accurate, precise and sensitive method has been developed for the simultaneous estimation of Furosemide and Spironolactone in their combined tablet dosage form. The method was carried out on a Hiber C₁₈ column (250 mm×4.6mm, i.d.5 μm) with a mobile phase consisting of acetonitrile: water at a flow rate of 1 ml/min and the detection was carried out at 237 nm. The retention time of Furosemide and Spironolactone was 3.81 min and 7.28 min. respectively. Linearity for Furosemide and Spironolactone were found in the range of 2-10 μg/ml and 5-25 μg/ml respectively. The developed method was validated in terms of linearity, accuracy, and precision, limit of detection (LOD) and limit of quantification (LOQ). The proposed method can be used for estimation of both drugs in their combined dosage form.

About Authors:
1) Mr Jaesh N.Jadhav
M.Pharm,Sinhagad Institute of pharmacy,Pune.
2) Mr. J.G. Chandorkar*.
Head Analytical development laboratory,
Indofil Industries limited,Thane
*Jayant.chandorkar@rediffmail.com

Abstract
A present work describes a simple & accurate reversed phase HPLC Method for the simultaneous estimation of Ortho Chlorophenol [OCP], 2,6 – Dichlorophenol [DCP], 1-(2,6-Dichlorophenyl) indolin-2-one [VTCL], 1(2,6-Dichlorophenyl) N-Phenyl, N-Chloro Acetyl, 2,6-Dichloro Aniline [VTDL], 1(2,6-Dichlorophenyl) ether [DCPE], 1(2,6-Dichlorophenyl) amine [DCPA] in Diclofenac Sodium bulk manufacturing. This paper describes a new rapid, easy Isocratic reversed phase HPLC method for the separation and estimation of six intermediates and Diclofenac Sodium. The primary purpose of this study is to compile HPLC data on the determination of these seven products, the compilation of such HPLC data being useful as reference guide.

About Authors:
Shah Chirag K.*, Umalkar Deepak, Dr. Rajesh KS.
Parul Institute of Pharmacy, Gujarat University,
Waghodia-391760, Dist. Vadodara,
Gujarat, India.
*cks2484@gmail.com

Abstract:
The present manuscript described the simple, rapid, accurate, sensitive, precise and economical Q- absorption ratio method for simultaneous determination of Cefixime and Moxifloxacin in combined tablet dosage form. Absorption ratio method uses the ratio of absorbances at selected wavelengths, one which is isoabsorptive point and other being the λ_max of the one of the components. Cefixime and Moxifloxacin shows isoabsorptive point at 275nm in 0.1N HCl. The second wavelength used is 295nm, which is λ_max of Moxifloxacin. The concentrations of the drugs were determined by using ratio of absorances at isoabsorptive point and at λ_max of Moxifloxacin. The method successfully applied to the Pharmaceutical formulation because no interference from the tablet formulation excipients was found. The results of analysis have been validated statistically and by recovery studies.

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About Authors:
T.R.PARTHASARATHI*, M.VANITHA SRI.
BIOANALYTICAL DEPARTMENT,
QUEST LIFE SCIENCES PVT. LTD, SDF III, MEPZ,
TAMBARAM, CHENNAI- 600 045, INDIA.
*parthu_14@yahoo.co.in

ABSTRACT :
A novel isocratic reverse-phase high performance liquid-chromatography method for determination of asenapine maleate was developed and validated after optimization of various chromatographic conditions. Samples were separated on a waters x-terra C₁₈ (100 mm × 4.6 mm, 3.5 μ) analytical column. The mobile phase used was acetonitrile: 0.1M phosphate buffer (p^H 3.2) 65:35%v/v operated at 30 °C column oven temperature was pumped at a flow rate of 1.0 mL min⁻¹ and the column eluents were monitored at a wavelength of 272 nm. When sample was injected into the Finnigan surveyor high performance liquid-chromatography system through Finnigan surveyor auto-sampler injector, separation was achieved within 5.0 min. The present method demonstrated was validated with the acceptable values for selectivity, linearity (within the expected concentration range (10–50 μg mL⁻¹; r² > 0.999)), recovery (>95%), precision (%RSD < 2.0), sensitivity (limit of detection: 1.85 µg mL⁻¹ and lower limit of quantification: 2.34 µg mL⁻¹), robustness, and ruggedness.

About authors:
Gourab Saha^*1, Pankaja Senapati¹, Narahari Sahu², Dr. Sambit Parida³
1. Department of Pharmaceutics, College of Pharmaceutical Sciences, Mohuda, Berhampur – 2, Orissa, India.
2. Department of Pharmacology, College of Pharmaceutical Sciences, Mohuda, Berhampur – 2, Orissa, India.
3. Department of Pharma analysis, College of Pharmaceutical Sciences, Mohuda, Berhampur–2, Orissa, India.
*gourab.pharma2012@gmail.com

Abstract
This study investigated the anti-inflammatory activity of the methanolic extract of Cissampelos pareira (Abuta) in male albino rats after intramuscular administration. This was done using the carragenin-induced paw edema method. Methanolic extract of Cissampelos pareira showed significant anti-inflammatory activity similar to ibuprofen and indomethacin.

About Authors:
Megana.H.S*, A.Satish Kumar Shetty, Anil Kumar S.M
*Department of Pharmaceutical Analysis,
National College of Pharmacy, Balraj Urs road,
Shimoga-577201,
Karnataka, India.
megana.leo@gmail.com

ABSTRACT
A novel, accurate, precise, sensitive, economic and rapid spectrophotometric methods has been developed and validated for simultaneous estimation of Triamterene and Benzthiazide in bulk and pharmaceutical dosage form. Triamterene and Benzthiazide showed absorption maxima at 363 nm and 283 nm in ethanol, which is used as solvent. In the present study, Area Under Curve method (Method A) developed, employedthe measurement of area at selected analytical wavelength ranges. Two analytical wavelength ranges selected were 358nm to 368nm nm (lmax of Triamterene is 363nm) and 278nm to 288nm (lmax of Benzthiazide is 283nm) for the estimation of Triamterene and Benzthiazide respectively.  Ratio derivative method (Method B) employed the measurement of amplitudes of Triamterene and Benzthiazide at their respective selected wavelengths. Two wavelengths selected were 359.2 nm and 300.4 nmfor the estimation of Triamterene and Benzthiazide respectivelybased upon divisor method.  Linearity was observed in the concentration range of 6-30 μg/ml and 3-15 μg/ml for Triamterene and Benzthiazide respectively. The recovery studies ascertained the accuracy of the proposed method and the results were validated as per ICH guidelines.

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.