scholarly journals Validation Thin Layer Chromatography for the Determination of Acetaminophen in Tablets and Comparison with a Pharmacopeial Method

2013 ◽  
Vol 2013 ◽  
pp. 1-10 ◽  
Author(s):  
Alina Pyka ◽  
Marika Budzisz ◽  
Małgorzata Dołowy
Keyword(s):  
Detection Limit ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Spectrophotometric Method ◽  
Commercial Products ◽  
Pharmaceutical Tablets ◽  
Related Substances ◽  
Quantity Control ◽  
Layer Chromatography

Adsorption thin layer chromatography (NP-TLC) with densitometry has been established for the identification and the quantification of acetaminophen in three leading commercial products of pharmaceutical tablets coded as brand: P1 (Productno. 1), P2 (Productno. 2), and P3 (Productno. 3). Applied chromatographic conditions have separated acetaminophen from its related substances, namely, 4-aminophenol and and 4′-chloroacetanilide. UV densitometry was performed in absorbance mode at 248 nm. The presented method was validated by specificity, range, linearity, accuracy, precision, detection limit, quantitative limit, and robustness. The TLC-densitometric method was also compared with a pharmacopeial UV-spectrophotometric method for the assay of acetaminophen, and the results confirmed statistically that the NP-TLC-densitometric method can be used as a substitute method. It could be said that the validated NP-TLC-densitometric method is suitable for the routine analysis of acetaminophen in quantity control laboratories.

Comparison of Postcolumn Derivatization-Liquid Chromatography with Thin-Layer Chromatography for Determination of Aflatoxins in Naturally Contaminated Corn

1990 ◽  
Vol 73 (4) ◽  
pp. 579-581 ◽  
Author(s):  
Rodney W Beaver ◽  
David M Wilson ◽  
Mary W Trucksess
Keyword(s):  
Liquid Chromatography ◽  
Detection Limit ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Correlation Coefficient ◽  
Low Levels ◽  
Aflatoxin B2 ◽  
Layer Chromatography ◽  
Postcolumn Derivatization

Abstract Quantitation of aflatoxins by liquid chromatography with postcolumn iodine derlvatization (LC-PCD) and fluorescence detection was compared with quantitation by the AOAC CB method, 968.22. Thirty-seven naturally contaminated corn samples were ground and then divided. One portion was extracted, and the extract was cleaned up and analyzed by thin-layer chromatography according to the CB method. The second portion was extracted and cleaned up In a similar fashion, but quantitation was by the LC-PCD method. For aflatoxin B1, concentrations ranging from 0 to 150 ng/g, results obtained by the 2 methods were fitted to a linear equation with the LC-PCD results as the dependent variable. The correlation coefficient was 0.99, the Intercept was near 0, and the slope was near 1. For aflatoxin B2, the correlation coefficient was 0.97, and the Intercept was near 0. However, the slope of the equation relating LC-PCD concentration to TLC concentration was only 0.5. We believe that this lack of equivalence between the methods for determination of aflatoxin B2 is due to overestlmatlon by the TLC method because the low levels present are near the TLC detection limit for B2.

Immunochromatography of Fusarochromanone Mycotoxins

1991 ◽  
Vol 74 (4) ◽  
pp. 655-660 ◽  
Author(s):  
Jaehyuk Yu ◽  
Fun Sun Chu
Keyword(s):  
Liquid Chromatography ◽  
Detection Limit ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Analytical Recovery ◽  
Layer Chromatography ◽  
Fungal Extracts

Abstract The present paper describes an enzyme-linked immunoassay (ELISA) used In combination with thin-layer chromatography (TLC) and liquid chromatography (LC) for determination of fusarochromanone (TDP) mycotoxins in barley, wheat, and a Fusarlum culture grown in rice and corn. The mycotoxins were first extracted from the sample with 100% methanol and subjected to TLC or LC without additional cleanup treatment. Individual fractions eluted from TLC or LC were acetylated, then analyzed by ELISA. Determinations of TDP toxins at levels as low as 0.1 and 0.5 ng were achieved by ELISA in combination with LC and TLC, respectively. The detection limit for TDP-1 in barley and wheat was about 20 ppb by ELISA alone as compared with a detection limit of 5 ppb by a combination of ELISA with either TLC or LC. Overall analytical recovery (% of added) of TDP-1 added to barley and wheat at 5,10, and 20 ppb of TDP-1 was 106.9 ± 15.3 and 113.2 ± 11.6 by LC-ELISA and 108.8 ± 9.1 and 110.4 ± 4.9 by TLC-ELISA, respectively. Analysis of extracts obtained from Fusarlum equiseti R6137 grown in corn and rice by the combination of TLC and ELISA revealed that diacetyl-TDP was also produced by this fungus in addition to TDP-1 and TDP-2. Comparable results were obtained when fungal extracts were subjected to ELISA, LC, and immunochromatography (i.e., combination of ELISA with either TLC or LC).

scholarly journals Dihydrochalcones and Chalcones of Some Flavanone Glycosides: Qualitativeand Quantitative Determinations

1975 ◽  
Vol 30 (11-12) ◽  
pp. 940-942 ◽  
Author(s):  
Harald A. B. Linke ◽  
Douglas E. Eveleigh
Keyword(s):  
Thin Layer ◽  
Quantitative Determination ◽  
Thin Layer Chromatography ◽  
Spectrophotometric Method ◽  
Detection Method ◽  
Alcoholic Solution ◽  
Agar Media ◽  
Layer Chromatography

The chalcones and dihydrochalcones of the flavanone glycosides naringin, neohesperidin and hesperidin were separated and identified by thin-layer chromatography; a similar procedure was utilized to perform preparative TLC for purification of these compounds. A new spectrophotometric method for the quantitative determination of dihydrochalcones in the concentration range from 0.005 to 0.100% in aqueous or alcoholic solution is described as well as a detection method of these compounds in agar media for microbiological studies.

Innovative Thin-Layer Chromatography/Fluorescence Detection Approach for Sensitive and Specific Determination of Ledipasvir in Rats’ Feces and Pharmaceutical Dosage Form

2021 ◽  
Author(s):  
Mohamed A Abdel-Lateef ◽  
Mahmoud A Omar ◽  
Ramadan Ali ◽  
Albandary Almahri ◽  
Sayed M Derayea
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Fluorescence Detection ◽  
Fecal Excretion ◽  
Content Uniformity ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Tablets ◽  
Specific Determination ◽  
Layer Chromatography

Abstract An innovative thin-layer chromatography method coupled with the fluorescence detection was developed for a specific estimation of ledipasvir. The separation was achieved on plates of silica gel 60 F254 using ethylacetate: hexane: acetonitrile: triethylamine; (6: 3.5: 1.5: 0.5, $\mathrm{v}/\mathrm{v}/\mathrm{v}/\mathrm{v}$) as a mobile phase system. The method involved the exposure of the developed thin-layer chromatography plate of ledipasvir to strong ultraviolet irradiation, resulting in a great enhancement in the fluorescence properties of ledipasvir. The irradiated plates were scanned after the excitation at 315 $\mathrm{nm}$. The method provided a sufficient separation of ledipasvir from sofosbuvir with ${R}_F$values of 0.28 and 0.36 for ledipasvir and sofosbuvir, respectively. The developed procedures were validated based on guidelines from the International Conference on Harmonization and Food and Drug Administration guidelines. The calibration curve was linear over the range of 5–50 $\mathrm{ng}/\mathrm{band}$. The excellent analytical features of the proposed method allow to the specific determination of ledipasvir in pharmaceutical tablets without interference from sofosbuvir or excipients. As the main elimination route for ledipasvir is via the fecal excretion (86%), the method was applied for the estimation of ledipasvir in fecal specimens with adequate recovery. In addition, the proposed method was applied for testing the content uniformity of ledipasvir in the pharmaceutical tablets.

Determination of Cyclopiazonic Acid in Peanuts and Corn by Thin Layer Chromatography

1986 ◽  
Vol 69 (6) ◽  
pp. 964-966 ◽  
Author(s):  
John A Lansden
Keyword(s):  
Detection Limit ◽  
Sodium Bicarbonate ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Cyclopiazonic Acid ◽  
Chromatographic System ◽  
Aqueous Sodium ◽  
Absolute Detection Limit ◽  
Layer Chromatography

Abstract A thin layer chromatographic system including densitometry has been developed for determining cyclopiazonic acid in peanuts and corn. Samples are extracted with methanol-chloroform (20 + 80); the extract is stripped of most interferences by partitioning with aqueous sodium bicarbonate followed by acidification and repartitioning with chloroform. After thin layer chromatography and derivatization with dimethylaminobenzaldehyde- HCl spray, the toxin is quantitated by reflection densitometry at 540 nm. The recovery of cyclopiazonic acid averages 90% for peanuts and 85% for corn. The absolute detection limit is 25 ng per spot which translates to a detection limit of 125 μg/kg for a 50 g sample.

scholarly journals Determination of curcumin in bouillon cubes by high-performance thin-layer chromatography

2021 ◽  
Vol 20 (66) ◽  
pp. 4-14
Author(s):  
A Yegorova ◽  
◽  
Yu Loskutova ◽  
G Voitiuk ◽  
A Maltsev ◽  
...  
Keyword(s):  
Detection Limit ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Calibration Curve ◽  
High Performance ◽  
Food Industries ◽  
Method Accuracy ◽  
First Time ◽  
Layer Chromatography

Currently, high-performance thin-layer chromatography (HPTLC) is widely used to control product quality in the pharmaceutical and food industries. In the manufacture of food products, the most important requirement is the control of the content of various additives (preservatives, dyes, antioxidants). For the first time, a method for determining curcumin by high-performance thin-layer chromatography in bouillon cubes "Gallina Blanca" was proposed. Detection was carried out by densitometric scanning using CAMAG equipment when measuring absorbance at a wavelength 265 nm. The method is based on determining the peak area of curcumin in the chromatogram depending on its concentration. Curcumin content is determined by the calibration curve. The developed method was validated by the following tests: specificity, linearity, accuracy and detection limit. The calibration curve is linear in the range of curcumin concentrations from 120 to 520 ng/spot, the detection limit is 65 ng/spot. The specificity of the method is based on the ability to unambiguously evaluate the analyte in the presence of other components and is confirmed by using an external standard. The spots on the chromatograms of the test solution and the reference solution coincide in the value of Rf, which confirms the specificity of the method. Accuracy was evaluated according to the results of the analysis of various samples. The requirement for statistical insignificance of systematic error is fulfilled. The proposed method is express, characterized by satisfactory metrological characteristics, ease of implementation. Key words: high-performance thin-layer chromatography, curcumin, validation.

scholarly journals Occurrence of Aflatoxins in Retail Kola Nuts in Ibadan Metropolis

2021 ◽  
pp. 1-5
Author(s):  
O. O. Akande ◽  
O. O. Kolawole ◽  
A. A. Afolabi ◽  
S. A. Okewole ◽  
L. O. Oyekunle
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Study Design ◽  
Aflatoxin B1 ◽  
Spectrophotometric Method ◽  
Layer Chromatography

Aim: This study was designed to determine Aflatoxins present in kola nuts sold in Ibadan metropolis. Study design: Kola nuts were randomly purchased from different markets in Ibadan, Oyo State. Methodology: Thin layer chromatography (TLC) and spectrophotometric method were used for the determination of aflatoxins in the kola nuts samples. Results: All the samples collected were contaminated with aflatoxins. Aflatoxin B1 and B2 were present in the kola nuts samples ranging from 9.73 - 25.43 μg/kg and 10.90 - 29.67 μg/kg respectively. Conclusion: The levels of aflatoxins in the sampled kola nuts were mostly above recommended tolerable limits. It is imperative to enlighten stakeholders on possible ways of handling kola nuts towards reducing the aflatoxin incidences to the barest minimum in order to safeguard the health of the populace.

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