Quantitation of Sulfamethazine in Pork Tissue by Thin-Layer Chromatography

1993 ◽  
Vol 76 (2) ◽  
pp. 335-341 ◽  
Author(s):  
Joseph Unruh ◽  
Daniel P Schwartz ◽  
Robert A Barford
Keyword(s):  
Thin Layer ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Signal To Noise Ratio ◽  
Internal Standard ◽  
Signal To Noise ◽  
Thin Layer Chromatographic Plate ◽  
Average Accuracy ◽  
Chromatographic Plate ◽  
Layer Chromatography

Abstract Our earlier method to detect and quantitate sulfamethazine (SMZ) in milk at the 10 ppb level was modified to quantitate SMZ in pork tissue. Sulfabromomethazine (SBZ) is added to the tissue as an internal standard. SMZ and SBZ are extracted from the tissue into water as the supernatant of a centrifuged, aqueous homogenate and are cleaned up and concentrated by a series of solid-phase extractions. The sulfonamide-containing eluate is then separated on a silica gel thin-layer chromatographic plate. SBZ and SMZ are derivatized with fluorescamine, and their fluorescence is quantitated with a scanning densitometer. The limit of detection was estimated at 0.25 ppb (signal-to-noise ratio, 3:1). The average accuracy over the analysis range (0.54-21.8 ppb [μg/kg]) was 95.6% (standard deviation = 29.4%, n = 54).

Laser-Based Photoacoustic Densitometer for Two-Dimensional Scanning of Thin-Layer Chromatographic Plates

1989 ◽  
Vol 43 (2) ◽  
pp. 249-253 ◽  
Author(s):  
Hirofumi Kawazumi ◽  
Edward S. Yeung
Keyword(s):  
Thin Layer ◽  
Spatial Resolution ◽  
Two Dimensional ◽  
Thin Layer Chromatographic Plate ◽  
Rapid Scan ◽  
Scan Time ◽  
Acousto Optic Device ◽  
Chromatographic Plate ◽  
Layer Chromatography ◽  
Scan Modes

Laser-based photoacoustic densitometry was applied to two-dimensional analysis in thin-layer chromatography. An acousto-optic device was used to provide both intensity modulation and a rastering scan. The spatial resolution is 25 × 60 spots for an area of 25 × 50 mm on the thin-layer chromatographic plate. Three detection modes, normal modulation, resonant modulation, and unmodulated rapid scan modes were compared. Detection limits in the most sensitive mode and in the fastest mode are 350 pg with scan time of 153 s and 6.9 ng with scan time of 1.5 s, respectively.

scholarly journals Method Development and Validation for Simultaneous Quantification of Microcystin Congeners in Water

2021 ◽  
Author(s):  
Xiaocui Qiao ◽  
Simin Ge ◽  
Chengyou Liu ◽  
Lixin Jiao ◽  
Xue Li ◽  
...  
Keyword(s):  
Formic Acid ◽  
Method Development ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Signal To Noise Ratio ◽  
Internal Standard ◽  
Ultra Performance Liquid Chromatography ◽  
Chaohu Lake ◽  
Online Spe ◽  
Relative Standard

Abstract Background: Microcystins, as secondary metabolites of cyanobacteria, are hepatotoxic to humans through the ingestion of cyanobacteria-contaminated water. Microcystins with diverse congeners in water can be precisely quantified using online solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (online-SPE UPLC-MS/MS). A method was developed and validated to simultaneously quantify eight microcystin congeners in water using online-SPE UPLC-MS/MS.Results: The method achieved the highest efficiency and sensitivity by selecting acetonitrile with 0.1% formic acid and water with 0.1% formic acid as the best mobile phase conditions. Linearity, accuracy, and precision were validated on matrix-mixed water with the leucine enkephalin internal standard. The limit of detection calculated using the signal-to-noise ratio of 3 passed the surface water daily inspection for microcystins. Except for the lower recovery of individual substances at individual concentrations, the recoveries of the remaining microcystin congeners ranged from 70 to 130%, and the relative standard deviation was less than 10%.Conclusion: The method was used to analyze microcystins in 12 water samples collected from Chaohu Lake. The sum of all microcystin congeners ranged from 101 to 585 ng L-1 in water (<WHO drinking water safe limit of 1 μg L-1 for microcystin-LR).

scholarly journals DETERMINATION OF 10-GINGEROL IN INDIAN GINGER BY VALIDATED HPTLC METHOD OF SAMPLES COLLECTED ACROSS SUBCONTINENT OF INDIA

2016 ◽  
Vol 8 (12) ◽  
pp. 190
Author(s):  
Kamran Ashraf ◽  
Syed Adnan Ali Shah ◽  
Mohd Mujeeb
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Aluminum Plates ◽  
Layer Chromatography ◽  
Hptlc Method

<p><strong>Objective: </strong>A simple, sensitive, precise, and accurate stability indicating HPTLC (high-performance thin-layer chromatography) method for analysis of 10-gingerol in ginger has been developed and validated as perICH guidelines.</p><p><strong>Methods: </strong>The separation was achieved on TLC (thin layer chromatography) aluminum plates pre-coated with silica gel 60F<sub>254</sub> using n-hexane: ethyl acetate 55:45 (%, v/v) as a mobile phase. Densitometric analysis was performed at 569 nm.</p><p><strong>Results: </strong>This system was found to have a compact spot of 10-gingerol at <em>R</em><sub>F</sub> value of 0.57±0.03. For the proposed procedure, linearity (<em>r</em><sup>2</sup> = 0.998±0.02), limit of detection (18ng/spot), limit of quantification (42 ng/spot), recovery (ranging from 98.35%–100.68%), were found to be satisfactory.</p><p><strong>Conclusion: </strong>Statistical analysis reveals that the content of 10-gingerol in different geographical region varied significantly. The highest and lowest concentration of 10-gingerol in ginger was found to be present in a sample of Patna, Lucknow and Surat respectively which inferred that the variety of ginger found in Patna, Lucknow are much superior to other regions of India.</p>

Development of a solid-phase extraction – spectrofluorimetric method for trace glutathione determination

2011 ◽  
Vol 89 (4) ◽  
pp. 517-523 ◽  
Author(s):  
Ke-Jing Huang ◽  
Cong-Hui Han ◽  
Ying-Ying Wu ◽  
Chao-Qun Han ◽  
De-Jun Niu ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Signal To Noise Ratio ◽  
Calibration Graph ◽  
Extraction Column ◽  
Phase Extraction ◽  
Selective Reaction ◽  
Spectrofluorimetric Method ◽  
Relative Standard

A simple and efficient solid-phase extraction – spectrofluorimetric method has been developed to determine glutathione (GSH). Fluorescent probe N-(4,4-difluoro-5,7-dimethyl-4-bora-3a,4a-diaza-s-indacene-3-yl)methyl)iodoacetamide (BODIPY Fl-C1-IA) was used as the derivatization reagent. The procedure was based on a BODIPY Fl-C1-IA selective reaction with GSH to form the highly fluorescent product BODIPY Fl-C1-IA–GSH, using a solid-phase extraction column and spectrofluorimetric determination. The variables affecting analytical performance were studied and optimized. The calibration graph using the preconcentration system for GSH was linear over the range of 1–200 nmol/L with a limit of detection of 0.05 nmol/L (signal-to-noise ratio = 3). The relative standard deviation for six replicate determinations of GSH at the 100 nmol/L concentration level was 3.9%. The method was applied to water samples and average recoveries between 87.5% and 111.5% were obtained for spiked samples.

Rapid Thin Layer Chromatographic Determination of Aflatoxin M1 in Powdered Milk

1985 ◽  
Vol 68 (5) ◽  
pp. 952-954
Author(s):  
Maria Luisa Serralheiro ◽  
Maria Lurdes Quinta
Keyword(s):  
Aqueous Solution ◽  
Carbon Tetrachloride ◽  
Thin Layer ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Methanol Solution ◽  
Aflatoxin M1 ◽  
Powdered Milk ◽  
Layer Chromatography

Abstract A method has been developed for the detection of aflatoxin Mi in milk. The toxin is extracted with chloroform, the extract is evaporated, and the residue is partitioned between carbon tetrachloride and an aqueous saline-methanol solution. The toxin is once again extracted with chloroform from the methanol solution and analyzed by thin layer chromatography. The limit of detection of Mi in powdered milk is 0.5 μg/ kg; recoveries of added Mj are about 83%. The limit of detection can be improved to 0.3 μg/kg if the plate is sprayed with an aqueous solution of H2S04 after development.

scholarly journals Sensitive Analysis of Idarubicin in Human Urine and Plasma by Liquid Chromatography with Fluorescence Detection: An Application in Drug Monitoring

Molecules ◽  
2020 ◽  
Vol 25 (24) ◽  
pp. 5799
Author(s):  
Olga Maliszewska ◽  
Natalia Treder ◽  
IIona Olędzka ◽  
Piotr Kowalski ◽  
Natalia Miękus ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Human Plasma ◽  
Fluorescence Detection ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Biological Fluids ◽  
Internal Standard ◽  
Urine Samples ◽  
Human Plasma And Urine ◽  
Plasma And Urine Samples

A new approach for the sensitive, robust and rapid determination of idarubicin (IDA) in human plasma and urine samples based on liquid chromatography with fluorescence detection (LC-FL) was developed. Satisfactory chromatographic separation of the analyte after solid-phase extraction (SPE) was performed on a Discovery HS C18 analytical column using a mixture of acetonitrile and 0.1% formic acid in water as the mobile phase in isocratic mode. IDA and daunorubicin hydrochloride used as an internal standard (I.S.) were monitored at the excitation and emission wavelengths of 487 and 547 nm, respectively. The method was validated according to the FDA and ICH guidelines. The linearity was confirmed in the range of 0.1–50 ng/mL and 0.25–200 ng/mL, while the limit of detection (LOD) was 0.05 and 0.125 ng/mL in plasma and urine samples, respectively. The developed LC-FL method was successfully applied for drug determinations in human plasma and urine after oral administration of IDA at a dose of 10 mg to a patient with highly advanced alveolar rhabdomyosarcoma (RMA). Moreover, the potential exposure to IDA present in both fluids for healthcare workers and the caregivers of patients has been evaluated. The present LC-FL method can be a useful tool in pharmacokinetic and clinical investigations, in the monitoring of chemotherapy containing IDA, as well as for sensitive and reliable IDA quantitation in biological fluids.

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