Application of Densitometry for the Evaluation of the Separation Effect of Nicotinic Acid Derivatives. Part I. Nicotinic Acid and its Amides

Pyka, Alina; Klimczok, W.

doi:10.1080/10826070701451670

Cited by 8 publications

(7 citation statements)

References 11 publications

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“…In the present paper, an attempt has been made to develop and validate a new, simple, cost-effective, and accurate RPHPTLC-densitometric method for accurate determination of nicotinamide ( Vitamin PP ) in both marketed formulations: tablets and injection solution. This work is continuation of previous extensive study by Pyka et al [ 45 – 50 ] concerning the use of TLC-densitometry in evaluation of chemical stability and also for the separation of various nicotinic acid derivatives. Numerous papers prepared by Pyka and coworkers affirmed that different mobile and also stationary phases including RP18WF 254 plates and TLC densitometry are suitable for the separation and to examine the chemical stability of these compounds [ 45 – 50 ].…”

Section: Resultssupporting

confidence: 69%

Validation of an RPHPTLC-Densitometric Method Using Silica Gel 60 RP18WF₂₅₄for Simultaneous Determination of Nicotinamide in Selected Pharmaceutical Formulations

Dołowy

Pyka

2015

Journal of Analytical Methods in Chemistry

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This research study describes the applicability of silica gel 60 RPW18F254 plates for the development and validation of new, simple, economic, accurate, and precise RPHPTLC-densitometric method suitable for the quantification of nicotinamide (as Vitamin PP) in three marketed preparations. The mobile phase used was methanol-water in volume composition 3 : 7. Detection wavelength was 200 nm. The proposed method was validated according to ICH guidelines and also based on Ferenczi-Fodor and Konieczka reports. Results were found to be linear over a range of 1.00 to 2.00 μg/spot. Limit of detection (LOD) and limit of quantification (LOQ) were 0.15 μg/spot and 0.45 μg/spot, respectively. The percent content of nicotinamide in the investigated preparations was found to be 99.2% (Product 1), 99.3% (Product 2), and 99.4% (Product 3). Developed method is accurate and precise (CV < 3%) and may be successfully applied for the quality control of pharmaceutical formulations containing nicotinamide in the presence of its derivatives, such as N,N-diethylnicotinamide, N-methylnicotinamide, and nicotinic acid.

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Section: Resultssupporting

confidence: 69%

Validation of an RPHPTLC-Densitometric Method Using Silica Gel 60 RP18WF₂₅₄for Simultaneous Determination of Nicotinamide in Selected Pharmaceutical Formulations

Dołowy

Pyka

2015

Journal of Analytical Methods in Chemistry

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“…Only densitometry provides an objective evaluation of the separation effect and the characteristics of particular chromatographic bands. The R S values obtained by the use of the visual method (R S(C) = 2 × d/s) were much higher than those obtained by densitometry [22,23]. Resolutions of peaks R S(b) , R S(h) , and R S(a) for the pair of compounds were calculated by use of eqs (4)- (6) at 254 nm in methanolwater mobile phase.…”

Section: Resultsmentioning

confidence: 89%

“…The obtained data are listed in Table I. For complete separation of neighboring compounds on a densitogram, R S must be greater than 1.5 [19,22,23]. The R S values greater than 1.5 were obtained over the entire range (10:0-6:4) of volume composition, except for E-TM where R S is much smaller than 1.0.…”

Section: Resultsmentioning

confidence: 98%

“…The R M values were then obtained using the equation R M = log(1/R F − 1) [16][17][18]. ∆R F , selectivity (α) [19][20][21], and the pair separation constant (R F α ) [21,22] were then calculated for all the densitograms by using eqs (1)- (3), respectively:…”

Section: Chromatographymentioning

confidence: 99%

“…The peak resolutions R S(b) [22][23][24] and R S(h) [22,23] were calculated using eqs (4) and (5), and the average peak resolution R S(a) was calculated using eq. (6):…”

Section: Chromatographymentioning

confidence: 99%

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Evaluation of separation parameters for selected organophosphorus fungicides of forensic importance by RP-HPTLC

Nagaraju¹,

Sanganalmath²,

Kemparaju

et al. 2012

Acta Chromatographica

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Summary.Studies on the evaluation of separation efficacies are of primary interest to forensic analysts for newly available pesticides. In the present work, a method is described for the separation evaluation of three selected organophosphorus fungicides (OPFs) ditalimfos (D), edifenfos (E), and tolclofos-methyl (TM) by reversed-phase high-performance thin-layer chromatography (RP-HPTLC). The method is based on the separation of three OPFs on silica gel 60 RP-18WF 254 plates with varying mobile phase compositions (10:0-6:4) of methanol-water. The relationship between the mobile phase composition and retention parameters (R F and R M ) as well as separation parameters (ΔR F , R S , α, R F α ) was analyzed. The three OPFs are completely separated from each other with ΔR F ≥ 0.04, except for the pair of compounds E-TM in the mobile phase composition 10:0, 7:3, 6.5:3.5, and 6:4. Under the chromatographic conditions used, TM was adsorbed the strongest, followed by E and D, which is indicated by the higher R M values obtained for TM. Peak resolution (R S ) values greater than 1.5 were obtained over the entire range of mobile phase composition, except for the pair of compounds E-TM. The UV apex of maximum absorption was 200 nm for all the three OPFs as measured by multiwavelength scan in the UV range, and higher values of peak area and peak height were obtained at the same wavelength. The present study clearly indicates that the system of RP-HPTLC with mobile phase methanol-water in a volume composition 8:2 (v/v) provides the optimum conditions for the separation of the three OPFs. However, the complete separation of E from TM was not achieved using this system.

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Gold nanoparticles grafted modified silica gel as a new stationary phase for separation and determination of steroid hormones by thin layer chromatography

Amoli‐Diva

Pourghazi

2015

Journal of Food and Drug Analysis

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A new thin layer chromatographic layer using gold nanoparticles grafted 3-triethoxysilyl propylamine modified silica gel (Au NPs-APTS modified silica gel) was developed as a stationary phase for separation and determination of two steroid hormones, namely progesterone and testosterone. Acetone-n-hexane 25:75 (v/v) was used as the mobile phase, and the results were compared with those obtained using plain (i.e., unmodified) silica gel plates. Some chromatographic parameters used for separation of the two steroids on an Au NPs-APTS modified silica gel plate as well as on a plain silica gel plate, including ΔR, separation factor (α), and resolution (R), were evaluated and compared. The reproducibility of R values was also determined by analysis of the two steroids in 7 consecutive days on both plates. Validity of the method was investigated, and a wide linear range of 1-200 ng per spot, and low detection limits of 0.16 ng and 0.13 ng per spot, low quantification limits of 0.51 ng and 0.40 ng per spot, and good precision (expressed as percent relative standard deviation) lower than 3.1% and 2.7% were obtained for progesterone and testosterone, respectively. As the results revealed, the proposed method is rapid and sensitive, and it is applicable to separation and determination of progesterone and testosterone in biological matrices such as urine samples.

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Application of Densitometry for the Evaluation of the Separation Effect of Nicotinic Acid Derivatives. Part I. Nicotinic Acid and its Amides

Cited by 8 publications

References 11 publications

Validation of an RPHPTLC-Densitometric Method Using Silica Gel 60 RP18WF₂₅₄for Simultaneous Determination of Nicotinamide in Selected Pharmaceutical Formulations

Validation of an RPHPTLC-Densitometric Method Using Silica Gel 60 RP18WF₂₅₄for Simultaneous Determination of Nicotinamide in Selected Pharmaceutical Formulations

Evaluation of separation parameters for selected organophosphorus fungicides of forensic importance by RP-HPTLC

Gold nanoparticles grafted modified silica gel as a new stationary phase for separation and determination of steroid hormones by thin layer chromatography

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Application of Densitometry for the Evaluation of the Separation Effect of Nicotinic Acid Derivatives. Part I. Nicotinic Acid and its Amides

Cited by 8 publications

References 11 publications

Validation of an RPHPTLC-Densitometric Method Using Silica Gel 60 RP18WF254for Simultaneous Determination of Nicotinamide in Selected Pharmaceutical Formulations

Validation of an RPHPTLC-Densitometric Method Using Silica Gel 60 RP18WF254for Simultaneous Determination of Nicotinamide in Selected Pharmaceutical Formulations

Evaluation of separation parameters for selected organophosphorus fungicides of forensic importance by RP-HPTLC

Gold nanoparticles grafted modified silica gel as a new stationary phase for separation and determination of steroid hormones by thin layer chromatography

Contact Info

Product

Resources

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Validation of an RPHPTLC-Densitometric Method Using Silica Gel 60 RP18WF₂₅₄for Simultaneous Determination of Nicotinamide in Selected Pharmaceutical Formulations

Validation of an RPHPTLC-Densitometric Method Using Silica Gel 60 RP18WF₂₅₄for Simultaneous Determination of Nicotinamide in Selected Pharmaceutical Formulations