A simple, economic, selective, precise, and stability-indicating high-performance thin-layer chromatographic method for analysis of tamsulosin hydrochloride, both as a bulk drug and in formulations, was developed and validated according to ICH guidelines. The method employed HPTLC aluminium plates precoated with silica gel 60F-254 as the stationary phase while the solvent system consisted of toluene&#x2009;&#x2009;:&#x2009;&#x2009;methanol&#x2009;&#x2009;:&#x2009;&#x2009;triethylamine (3.5&#x2009;&#x2009;:&#x2009;&#x2009;1.2&#x2009;&#x2009;:&#x2009;&#x2009;0.2&#x2009;v/v). The system was found to give compact spot for drug (<svg style="vertical-align:-4.28516pt;width:17.737499px;" id="M1" height="14.6125" version="1.1" viewBox="0 0 17.737499 14.6125" width="17.737499"  xmlns="http://www.w3.org/2000/svg"    >
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</svg>). Densitometric analysis of tamsulosin was carried out in the absorbance mode at 280&#x2009;nm. The linear regression analysis data for the calibration plots showed good linear relationship, <svg style="vertical-align:-1.58624pt;width:125.125px;" id="M3" height="14.3375" version="1.1" viewBox="0 0 125.125 14.3375" width="125.125"  xmlns="http://www.w3.org/2000/svg"    >
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				<tspan style="font-size: 11.21px; " x="0" y="0">=</tspan>
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</svg> with respect to peak area in the concentration range 400&#x2013;2400&#x2009;ng per spot. The mean value &#xb1; SD of slope and intercept were <svg style="vertical-align:-0.97874pt;width:97.675003px;" id="M4" height="10.9875" version="1.1" viewBox="0 0 97.675003 10.9875" width="97.675003"  xmlns="http://www.w3.org/2000/svg"    >
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			</text>

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				<tspan style="font-size: 11.21px; " x="55.614098" y="0">8</tspan>
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</svg> with respect to peak area. The method was validated for precision, recovery, and robustness. The limits of detection and quantitation were 20.49 and 62.10&#x2009;ng per spot, respectively. Tamsulosin was subjected to hydrolysis, oxidation, and thermal degradation which indicate the drug is susceptible to hydrolysis, oxidation, and heat. Statistical analysis proves that the method is repeatable, selective, and accurate for the estimation of tamsulosin.

S. B. Bari

A. R. Bakhshi

P. S. Jain

S. J. Surana

Development and Validation of Stability-Indicating HPTLC Determination of Tamsulosin in Bulk and Pharmaceutical Dosage Form

The ease of separation by gas chromatography between petroselinic and oleic acids depends on the alcohol moieties of their esters. The esters of higher molecular weight alcohols tend to be better separated on a 90%-biscyanopropyl-10%-cyanopropylphenyl polysiloxane capillary column (30 m × 0.25 mm i.d.). By analysis of free energies contribution from different parts of the molecules, it is tentatively concluded that the interaction between the double bond and the column stationary phase is interfered by the bulky alkyl group, and it is the major driving force for the separation of the two fatty acids.

Chanida Sansa-ard

Kornkanok Aryusuk

Supathra Lilitchan

Kanit Krisnangkura

Free Energy Contribution to Gas Chromatographic Separation of Petroselinate and Oleate Esters

Oscillatory reactions are a narrow reaction type among the entity of chemical reactions and those involving purely organic compounds make a small contribution to an overall number of all known oscillatory reactions. The most abundant type is purely inorganic and mixed inorganic-organic oxidation-reduction reactions, basically because monitoring them is relatively easy (e.g., with use of potentiometric measurements). Investigation of the organic reactions can be more demanding, and then chromatography is an analytical technique of choice. In this paper, we provide an overview of chromatographic evidence with oscillatory reactions discovered in our laboratory in the course of the last several years that involve the low-molecular-weight carboxylic acids (profen drugs, amino acids, and hydroxy acids). The investigated processes comprise the oscillatory chiral conversion and the oscillatory condensation, spontaneously running in the aqueous and nonaqueous abiotic media, and they were traced with use of TLC and HPLC coupled with different detector types.

Mieczyslaw Sajewicz

Teresa Kowalska

Liquid Chromatographic Investigation of Spontaneous Oscillatory <i>In Vitro</i> Chiral Conversion and Spontaneous Oscillatory Condensation of Simple Carboxylic Acids in Aqueous and Nonaqueous Media

We report a selective, accurate, and reproducible liquid chromatography-tandem mass spectrometric (LC-MS/MS) method that employs solid phase extraction for quantification of ketorolac enantiomers in human plasma. Resolution of R(+)-ketorolac and S(&#x2212;)-ketorolac was achieved using a Chiral-AGP column and a mobile phase of ammonium formate buffer (10&#x2009;mM, pH <svg style="vertical-align:-0.97874pt" id="M1" height="10.9875" version="1.1" viewBox="0 0 64.987503 10.9875" width="64.987503"  xmlns="http://www.w3.org/2000/svg"    >
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				<tspan style="font-size: 11.21px; " x="46.277832" y="0">5</tspan>
			</text>

		</g>
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</svg>):acetonitrile (85&#x2009;:&#x2009;15, v/v and 70&#x2009;:&#x2009;30, v/v) in a gradient time program. S(+)-etodolac was used as the internal standard (IS). Quantification was achieved using a positive electrospray ionization (ESI+) interface under multiple reaction monitoring (MRM) condition. The method was validated over the concentration range of 9.36&#x2013;1198.69&#x2009;ng/ml for R(+)-ketorolac and 6.07&#x2013;776.74&#x2009;ng/ml for S(&#x2212;)-ketorolac. Matrix effect was found negligible and the method showed good performances in terms of accuracy (89.6&#x2013;102.7&#x25;) and precision (1.7&#x2013;6.7&#x25;) for both enantiomers. 
Extraction recoveries of R(+)-ketorolac, S(&#x2212;)-ketorolac, and S(+)-etodolac were 82.04, 70.94, and 93.90&#x25;, respectively. Results of all stability exercises in human plasma were within acceptable limits. The method was successfully applied to a single dose cross over bioequivalence study in healthy human male volunteers. Incurred Sample Reanalysis (ISR) was performed by randomly selecting 10&#x25; of total subject samples of the study using Statistical Analysis Software (SAS). Values of 91.1&#x25; for R (+)-ketorolac and 83.5&#x25; for S(&#x2212;)-ketorolac indicated good acceptance for ISR.

Sabyasachi Patri

Anil K. Patni

Sunil S. Iyer

Arshad H. Khuroo

Tausif Monif

Sachin Rana

Sudershan Kumar

Rakesh Jain

A Validated High-Performance Liquid Chromatography-Tandem Mass Spectrometric (Lc-Ms/Ms) Method for Simultaneous Determination of R(+)-Ketorolac and S(&#x2212;)-Ketorolac in Human Plasma and Its Application to a Bioequivalence Study

A new, simple, and rapid stereoselective normal phase-liquid chromatographic (NP-LC) method was developed to separate and quantify the solifenacin succinate and its three stereoisomers. The stereoisomeric separation was achieved on Chiralpak IC (<svg style="vertical-align:-0.3135pt;width:60.049999px;" id="M1" height="11.2625" version="1.1" viewBox="0 0 60.049999 11.2625" width="60.049999"  xmlns="http://www.w3.org/2000/svg">
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				<tspan style="font-size: 12.50px; " x="21.530167" y="0">×</tspan>
				<tspan style="font-size: 12.50px; " x="32.307751" y="0">4</tspan>
				<tspan style="font-size: 12.50px; " x="38.559254" y="0">.</tspan>
				<tspan style="font-size: 12.50px; " x="41.685001" y="0">6</tspan>
			</text>

		</g>
	</g>
</svg>&#x2009;mm ID) column. The mobile phase was consisting of n-hexane, ethanol, isopropyl alcohol, and diethylamine in the ratio (60&#x2009;:&#x2009;15&#x2009;:&#x2009;25&#x2009;:&#x2009;0.1, v/v/v/v), and the flow rate was maintained at 1.0&#x2009;mL&#x2009;min<sup  >&#x2212;1</sup>. UV detection was carried out at 220&#x2009;nm. In addition, chiroptical detection was carried out using laser polarimeter to understand the elution orders. Resolution between all the stereoisomers was not less than 3. Effect of column temperature on resolution between the stereoisomers was studied. The method was validated as per ICH guideline and found to be robust. The proposed NP-LC method was successfully applied to the analysis of commercial formulation. The method could be of use not only for routine evaluation of the quality of solifenacin succinate in bulk drug manufacturing unit but also for detection of impurities in pharmaceutical formulations.

Shashikant B. Landge

Sanjay A. Jadhav

Sunil B. Dahale

Navanath C. Niphade

Ch. Lakshmi Narayana

Vishwas B. Gaikwad

Vijayavitthal T. Mathad

Development and Validation of New Chromatographic Method for the Determination of Enantiomeric and Diastereomeric Purity of Solifenacin Succinate: An Antimuscarinic Agent

A new, simple, and rapid high-performance thin-layer chromatographic method was developed and validated for quantitative determination of Carbamazepine. Carbamazepine was chromatographed on silica gel 60 <mml:math xmlns:mml="http://www.w3.org/1998/Math/MathML"><mml:mrow><mml:msub><mml:mtext>F</mml:mtext><mml:mrow><mml:mtext>254</mml:mtext></mml:mrow></mml:msub></mml:mrow></mml:math> TLC plate using ethyl acetate-toluene-methanol (5.0 + 4.0 + 1.0 v/v/v) as mobile phase. Carbamazepine was quantified by densitometric analysis at 285 nm. The method was found to give compact spots for the drug (<mml:math xmlns:mml="http://www.w3.org/1998/Math/MathML"><mml:mrow><mml:msub><mml:mi>R</mml:mi><mml:mi>f</mml:mi></mml:msub><mml:mo>=</mml:mo><mml:mn>0</mml:mn><mml:mo>.</mml:mo><mml:mn>47 </mml:mn></mml:mrow></mml:math><mml:math xmlns:mml="http://www.w3.org/1998/Math/MathML"><mml:mo>±</mml:mo></mml:math> 0.01). The linear regression analysis data for the calibration plots showed good linear relationship with <mml:math xmlns:mml="http://www.w3.org/1998/Math/MathML"><mml:mrow><mml:msup><mml:mi>r</mml:mi><mml:mn>2</mml:mn></mml:msup><mml:mo>=</mml:mo><mml:mn>.9995</mml:mn></mml:mrow></mml:math> in the concentration range 100–600 ng/spot. The method was validated for precision, recovery, repeatability, and robustness as per the International Conference on Harmonization guidelines. The minimum detectable amount was found to be 16.7 ng/spot, whereas the limit of quantitation was found to be 50.44 ng/spot. Statistical analysis of the data showed that the method is precise, accurate, reproducible, and selective for the analysis of Carbamazepine. The method was successfully employed for the estimation of equilibrium solubility, quantification of Carbamazepine as a bulk drug, in commercially available preparation, and in-house developed mucoadhesive microemulsion formulations and solution.

Rashmin B. Patel

Mrunali R. Patel

Kashyap K. Bhatt

Bharat G. Patel

Development and Validation of HPTLC Method for Estimation of Carbamazepine in Formulations and Its <i>In Vitro</i> Release Study

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Chromatography Research International - Table of contents 2011

Chromatography Research International | Hindawi

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