The standard solutions of CEF and LIN were scanned separately in the UV range and zero-order spectra for CEF and LIN were recorded. Maximum absorbance was obtained at 287.20 nm and 250.60 nm for CEF and LIN, respectively. These two wavelengths can be employed for the determination of CEF and LIN without any interference from the other drug in their combined synthetic mixture. Overlain zero-order absorption spectrum of CEF and LIN in methanol is shown in (Figure 3). Linear correlation was obtained between absorbances and concentrations of CEF and LIN in the concentration ranges of 2-22 µg/ml and 2-18 µg/ml, respectively. The linearity of the calibration curve was validated by the high values of correlation coefficient of regression. The RSD values of CEF were found to be 0.98 and 0.97 % at 287.20 and 250.60 nm, respectively. The RSD value of LIN was found to be 1.44 and 0.77 % at 287.20 and 250.60 nm, respectively. Relative standard deviation was less than 2 %, which indicates that proposed method is repeatable. The low RSD values of interday (0.47-0.91% and 0.46-0.86% for CEF at 287.20 and 250.60 nm, respectively and 0.77- 0.99% and 0.49-0.71% for LIN at 287.20and 250.60 nm, respectively) and intraday (0.58-0.95% and 0.53-1.07% for CEF at 287.20 and 250.60 nm, respectively and 0.86-1.49% and 0.51-0.82% for LIN at 287.20 and 250.60 nm, respectively) variation for CEF and LIN, reveal that the proposed method is precise. LOD and LOQ values for CEF were found to be 0.34 and 1.02 µg/ml and 0.38 and 1.14
The compound was identified by taking the IR spectra. The method is applied for laboratory mixture and marketed tablet. The developed method was validated as per ICH guidelines using the parameter such as accuracy, linearity and range, ruggedness, limit of detection & quantification, robustness, and precisión. Precisión was analysed by taking Reading interday and Intraday. Ruggedness was analysed by differant analyst and robustness by changing the solvent composition.
The proposed methods for simultaneousestimationof PARA, PHEN and CHLOR in combined dosageform were found to be accurate, simple and rapid which can be well understood from va1lidation data as given in Table 3 and 4. The % R.S.D. Linearity was observed by linear regression equation method for PARA, PHEN and CHLOR in different concentration range. The Correlation coefficient of these drugs was found to be close to 1.00, indicating good linearity. The assay results obtained by proposed methods as shown in Table 2, hence it can be used for routine analysis of two drugs in combined dosage forms. There was no interference from tablet excipients was observed in these methods. It can be easily and conveniently adopted for routine quality control analysis. These methods are accurate, simple, rapid, precise, reliable, sensitive, reproducible and economic and are validated as per ICH guidelines.
The present work represents a UV-Spectrophotometricmethod for the simultaneousestimationof Formoterol Fumarate (FF) and Mometasone Furoate (MF) in respicaps dosageform. This method is based on area under curve (AUC) in the wavelength range of 210-220nm and 242-252nm. Linearity was found in the concentration ranges of 3-18μg/ml and 6-21μg/ml, for Formoterol Fumarate and Mometasone Furoate, respectively. This method was validated as per International Conference on Harmonization (ICH) guidelines. Validation results suggest that the proposed method is simple, rapid, accurate, sensitive and precise that can be applied for routine estimationof FF and MF in bulk drug and combined dosageform.
Telmisartan (TEL) is an Angiotensin II receptor antagonist used an Antihypertensive drug [1-7]. chemically it is 4′-[[4-methyl-6-(1-methyl-2- benzimidazolyl)-2-propyl-1-benzimidazolyl]methyl]-2- biphenylcarboxylic acid (Figure.1). It is official in Indian Pharmacopoeia (IP), British Pharmacopoeia (BP) and U.S. Pharmacopoeia (USP). It is estimated by Liquid Chromatography as per IP and Potentiometric titration as per BP and USP [5- 7]. Literature review reveals that HPLC [8-12], UV [13-15] spectrophotometricand HPTLC [16-22] methods has been reported for estimationof TEL in pharmaceutical dosage forms.
2-(3-ethyl-4-methyl-2-oxo-3 pyrroline-1-carboxamido) ethyl- phenylsulfonyl-3-(trans-4-methylcyclohexyl) urea 8-11 . It is a medium to long acting sulphonyl urea anti-diabetic drug. Several spectrophotometricmethod, HPLC, HPTLC have been reported for estimationof Glimepiride 5-7 . Pioglitazone is one of the PPAR-alpha agonist, insulin sensitizer used to reduce the insulin resistance. It is a thiazolidine dione derivative and chemically (RS)-5-(4-[2-(5-ethylpyridin-2- yl)ethoxy]benzyl)thiazolidine-2,4-dione. HPLC and UV- visible spectrophotometry methods have been reported for its individual determination of Pioglitazone andin combination with other drugs. The present manuscript describes a novel LC method which is simple, rapid, precise, sensitive, selective and accurate isocratic reverse phase HPLC-UV method for simultaneous determination of metformin, pioglitazone and glimepiride intabletdosageform 8-10 .
Eperisone (EPE) is chemically 4-ethyl-2-methyle-3- piperidinopropiopenone (Figure 1) is a well known antispasmodic drug 1 . It is official in Japanese Pharmacopoeia (JP). JP 2 describe potentiometric method for its estimation. Literature survey reveals Electron spray Ionization Mass Spectroscopy for determination of Eperisone in human plasma. 3 The use of HPLC/MS, GC/MS, NMR, UV and IR to Identify Degredation product of eperisone hydrochloride in the the tablets. 4, Diclofenac sodium (DIC) is chemically 2-[2,6dichlorophenylamino] benzene acetic acid sodium salt 5 (Figure 2). Diclofenac sodium (DIC) is official in IP and BP. IP 6 and BP 7 describes liquid chromatography method for its estimation. Literature survey reveals HPTLC 8 and UV 13 , 14 methods for determination of DIC in single dosageform. Literature survey also reveals HPLC 9,11,12 , UV spectrophotometry 14 and HPTLC 15 method for the determination of DIC with other drugs in combination. The combination of these two drugs is not official in any pharmacopoeia; hence no official method is available for the simultaneousestimationof EPE and DIC in their combined dosage forms. Literature survey does not reveal any simple spectrophotometricmethod for simultaneousestimationof EPE and DIC in synthetic mixture or dosage forms. The present communication describes simple, sensitive, rapid, accurate, precise and cost effective spectrophotometricmethod based on simultaneous equations for simultaneousestimationof both drugs in their combined synthetic mixture. MATERIALS AND METHODS
18. Abdullah Al masud, Mohammad saydur rahman, moynul Hasan, Md.Kamal Hassain Ripon, Ahsanur Rahman Khan, Md.Rabiul Islam, Md.Monjurul Ahasan, Md.Rakib Uddin.Validated RP-HPLC methods for the simultaneous determination of Atorvastatin and Amlodipine intabletdosageform. Bangladesh Research Publications journal.september-october, 2011; 52-6
Introducing HPTLC into pharmaceutical analysis represents a major step in terms of quality assurance. Today HPTLC is rapidly becoming a routine analytical technique due to its advantages of low operating costs, high sample throughput and the need for minimum sample preparation. The major advantage of HPTLC is that several samples can be run simultaneously using a small quantity of mobile phase-unlike HPLC - thus reducing the analysis time and cost per analysis. The developed HPTLC technique is precise, specific and accurate. Statistical analysis proves that the method is suitable for the analysis of AMB and DES in pharmaceutical formulation without any interference from the excipients. The common excipients and other additives are usually present in the tabletdosageform do not interfere in the analysis of AMB and DES inmethod, hence it can be conveniently adopted for routine quality control.
Metaxalone, a muscle relaxant used to relax muscles and relieve pain caused by strains, sprains and othermusculoskeletal conditions. A simple, accurate, precise, reproducible, highly sensitive, economic UV spectrophotometricmethod has been developed for the estimationof metaxalon in bulk andtabletdosageform. In this method metaxalon showed maximum absorbance at 280 nm in methanol. The developed spectrophotometricmethod was validated in accordance with ICH guidelines. Linearity of the method was found to be 5 - 160µg/ml. The method obeyed Beer’s law in the concentration range of 5 -160 µg/ml. The LOD and LOQ were found to be 3.489μg/ml and 10.575μg/ml respectively. A mean recovery of metaxalon intabletdosageform was found to be 99.69%.the method was found to be simple, accurate, precise, specific, sensitive, reproducible and can be directly and easily applied to tabletdosageform.
Amlodipine besylate (AMLO) is chemically 3-ethyl 5-methyl (4RS)-2-[(2 aminoethoxy)methyl]-4-(2-chlorophenyl) 6- methyl-1,4 dihydropyridine-3,5-dicarboxylate benzenesulphonate 8 (Figure 1), is a Calcium channel blocker, used in the treatment of hypertension 9 . It is official in IP, BP and USP. IP 1 , BP 3 and USP 2 describe HPLC method for its estimation. Literature survey reveals UV spectrophotometry 4 , RP-HPLC 5 , spectrophotometric 6 method for simultaneous determination of AMLO with other drug and RP-HPLC 7 method for simultaneous determination of AMLO with other drug methods for determination of AMLO in pharmaceutical dosage forms as well as in biological fluids. Indapamide (INDA) is chemically 4-Chloro-N-[(2RS)-2-methyl-2,3- dihydro-1H-indol-1-yl]-3-sulphamoylbenzamide 18 (Figure 2), is a Thiazide diuretics for the treatment of hypertension 19 . Indapamide is official in IP 10 , BP 12 and USP 11 . IP, BP, and USP describe HPLC method for its estimation. Literature survey reveals LC-MS 13 , spectrophotometric 14 and HPLC 15 method for simultaneousestimationof INDA in whole human blood, RP-HPLC 16 method for simultaneousestimationof INDA, LC-ESI-MS 17 methods for the determination of INDA in human plasma. This combination is not official in any pharmacopoeia hence official and reported methods of analysis are not available for this combination. The present manuscript describes simple, sensitive, accurate, precise, rapid and economic First derivative spectrophotometricmethod for simultaneousestimationof AMLO and INDA intabletdosageform. MATERIALS AND METHODS
Metformin HCl (MET) is chemically N,N - dimethylimidodicarbonimidic diamide hydrochloride. Metformin improves hyperglycemia primarily through its suppression of hepatic glucose production. It activates AMP- activated protein kinase (AMPK), a liver enzyme that plays an important role in insulin signaling, whole body energy balance, and the metabolism of glucose and fats, activation of AMPK is required for metformin inhibitory effect on the production of glucose by liver cells. Activation of AMPK is required for an increase in the expression of SHP, which in turn inhibits the expression of the hepatic gluconeogenic genes PEPCK and Glc-6-Pase. Metformin increases the amount of cytosolic AMP. Metformin is contraindicated in people with any condition that could increase the risk of lactic acidosis, including kidney disorders, lung disease and liver disease 2 .
A simple, precise, accurate, sensitive and rapid Simultaneous Equation method was developed for simultaneousestimationof Cefuroxime Axetil(CEF) andLinezolid(LIN) inTabletdosageform. The proposed method was applied for the determination of Cefuroxime Axetil andLinezolidinTablet formulation, for determination of sampling using two wavelengths, CEF and LIN were scanned in 200-400 nm range and sampling wavelengths were 276.60 nm for CEF and 257.40 nm for LIN are selected for development and validation ofsimultaneous equation method. For this method linearity observed in the range of 2-6 μg/ml for CEF and 2.4-7.2 μ g/ml for LIN andin their pharmaceutical formulation with mean percentage recoveries 99.90± 0.005 and 100.02± 0.009, respectively. The method was validated according to ICH guidelines and can be applied for routine quality control testing.
Paracetamol (PCM) is N-(4-hydroxyphenyl) acetamide (Figure 1(a)) is a potent analgesic and anti-pyretic. It is generally used in the treatment of headache, toothache, backache, dysmenorrhea, myalgia and neuralgia. Aceclofenac (ACF) is 2-[2-[2-[(2,6-dichlorophenyl) amino] phenyl]acetyl]oxyacetic acid (Figure 1(b)) is the most widely used NSAID presently. The primary mechanism of action of diclofenac is inhibition of Cyclooxygenase (COX) enzyme leading to the inhibition of prostaglandin biosynthesis. It is used for the relief of pain and inflammation in rheumatoid arthritis, osteoarthritis, ankylosing spondylosis, toothache and dysmenorrhea. Tizanidine (TIZ) is 5-chloro-N-(4, 5-dihydro- 1H-imidazol-2-yl) benzo [c] [1,2,5] thia diazol-4-amine (Figure 1(c)) is a centrally acting skeletal muscle relaxant. It is a centrally acting α 2 adrenergic agonist
methods were also evaluated and compared with the reference HPLC methodin the dissolution proile test. Dissolution tests were carried out on tablets produced by the ive different manufacturers. To compare methods, a t-test was applied at each point of the dissolution proile. No statistically signiicant differences (at 95% conidence level) were found among the results of the methods. This result demonstrates that the derivative and PLS methods may be applied to an extended range of concentrations. Figure 3 shows the proile for laboratory A, as an example. For all methods, the similarity of the results is evident. Results from the irst sampling time showed a large variability due to the technological aspects inherent to the manufacturing process of tablets. Among these,
Twenty tablets were weighed and transferred intact to a 500 ml volumetric flask. About 300 ml of mobile phase was added and sonicated for 30 min after disintegration to effect complete dissolution of sodium valproate, cooled and the solutions were made up to volume with mobile phase. Aliquots of the solution were filtered through a 0.45 µm nylon filter and 5 ml of the filtered solution was transferred to a 100 ml volumetric flask and made up to volume with mobile phase. The solutions were injected at above chromatographic conditions and peak areas were measured to determine the sodium valproate content (Fig. 1).
[iminobis(methylene)]bis[6-fluoro-3,4-dihydro-2H-1- benzopyran-2-methanol] hydrochloride. It is a highly selective β1-blocker with nitric oxide mediated vasodilatory actions and beneficial effects on vascular endothelial function. Nebivolol is used in the management of hypertension. [1-2] Various analytical methods have been reported for determination of nebivolol including UV spectrophotometry [3] , HPLC [4-10] , LC-MS [11] , HPTLC [12-14] . Hydrochlorothiazide (HCTZ) is chemically known as 6- chloro-3,4-dihydro-7-sulfamoyl-2H-1,2,4-benzothiadiazine- 1,1-dioxide. It is a thiazide diuretic & increases sodium and chloride excretion in distal convoluted tubule. Literature survey reveals that few UV [15-17] and HPLC [18-21] methods have been reported for determination of hydrochlorothiazide. The combination of NBV and HCTZ is choice for treatment of many low rennin hypertensions. Some methods are reported for the combination of Nebivolol and Hydrochlorothiazide including UV [22-24] , HPLC [25-26] and HPTLC [27] . The purpose of this investigation was to develop
A simple, selective, accurate high Performance Liquid Chromatographic (HPLC) method was developed and validated for the analysis of Sexagliptin and Pioglitazone. Chromatographic separation achieved isocratically on a C18 column [Use Inertsil C18, 5m , 150 mm x 4.6 mm] utilizing a mobile phase of acetonitrile/phosphate buffer (60:40, v/v, pH 7.0) at a flow rate of 0.8 ml/min with UV detection at 260nm.Aceclofenac was used as an internal standard. The retention time of Sexagliptin, pioglitazone and aceclofenac was 2.48, 4.45 and 6.34 min respectively. The developed method was validated in terms of accuracy, precision, linearity, limit of detection, limit of quantitation.This study aimed at developing and validating an HPLC method, being simple, accurate and selective, and the proposed method can be used for the estimationof these drugs in combined dosage forms
Laboratory-prepared mixtures containing different ratios of PRO and HCT were prepared. By applying the procedure under linearity, absorbance at 289.0 nm was recorded for PRO and 270.0 nm were recorded for HCT. The concentration of each drug in each mixture was calculated from its corresponding Cx and Cy equation. Validity of the method was assessed by spiking the pharmaceutical formulation by known amounts of standard drug powders (standard addition technique). The recovery of the added standards was then calculated after applying the proposed method.
Checking the dependency of attributes is done to omit the un- necessary attributes, the step which can be of crucial importance in optimising the decision-making process. A smaller number of attributes means less of a dialogue with the user and quicker search of the rule base looking for adequate procedure of reason- ing. In the case of decision tables that contain very large sets of redundant attributes (created during the operations associated with data mining), the possibilities of reduction can become critical elements in building of a knowledge base. A totally different situation occurs when the decision table is created by knowledge engineers in a controlled manner, based on e.g. literature, expert knowledge, and/or standards, when the set of attributes is authori- tatively created basing on the available knowledge about the phenomena. In this case, the reduction of attributes is not neces- sary, as it can be assumed that the number of unnecessary attributes (if any) shall not deteriorate the model classificability.