CIRCULAR PAPER CHROMATOGRAPHIC METHOD FOR DETERMINING TRACE AMOUNTS OF COBALT, COPPER, NICKEL, AND ZINC IN ROCKS AND SOILS

1965 ◽  
Vol 2 (2) ◽  
pp. 33-43 ◽  
Author(s):  
D. C. Mah ◽  
S. Mah ◽  
W. M. Tupper
Keyword(s):  
Acid Solution ◽  
Paper Chromatography ◽  
Chloric Acid Solution ◽  
Rubeanic Acid ◽  
Circular Paper ◽  
Color Indicator ◽  
Higher Sensitivity ◽  
Circular Chromatography ◽  
Cobalt Copper

Ascending, descending, and horizontal (circular) methods of paper chromatography were explored and compared. Circular chromatography was found to be the most suitable; it requires shorter development time, has more definite Rf values, less tailing, higher sensitivity, and better precision than ascending or descending methods.A methyl ethyl ketone: hydrochloric acid solution (93:7 v/v) is used as a developing solvent for cobalt, copper, and nickel, and a 1-butanol: 1 N hydro–chloric acid solution (7:3 v/v) is used as a solvent for zinc. Good separations were obtained with these solvents and no critical interferences were noted. Benzidine – rubeanic acid is used as a color indicator for cobalt, copper, and nickel; and dithizone (0.01%) for zinc. This method has an absolute sensitivity of 0.005 μg for zinc, and 0.02 μg for cobalt, copper, and nickel. Precision is estimated at ± 10%.Methods have also been developed for determining bismuth, silver, and tin.The separation of elements from complex mixtures by paper chromatography and by quantitative determination of the amounts present by emission spectrography have been investigated. This rarely considered process offers promise, because the sensitivity of several elements is higher in emission spectrography than in colorimetry.

Simultaneous Determination of Alogliptin, Linagliptin, Saxagliptin, and Sitagliptin in Bulk Drug and Formulation by UPLC Q-TOF-MS

2020 ◽  
Vol 17 (1) ◽  
pp. 95-105
Author(s):  
Ramji Rathod ◽  
Faraat Ali ◽  
Amrish Chandra ◽  
Robin Kumar ◽  
Meenakshi Dahiya ◽  
...  
Keyword(s):  
Internal Standard ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Pharmaceutical Dosage Forms ◽  
Sensitivity And Selectivity ◽  
The Mean ◽  
Bulk Drug ◽  
Positive Ion ◽  
Higher Sensitivity

Background: A simple and sensitive Ultra Performance Liquid Chromatography-Mass Spectrometry method was developed and validated to measure the concentrations of Alogliptin (ALO), Linagliptin (LIN), Saxagliptin (SAX), and Sitagliptin (SIT) using Pioglitazone (PIO) as an internal standard. Methods: Chromatographic separation of six gliptins was achieved on a C-18 column (100×2.1 mm, 2.7 μm) using a mobile phase consisting of formic acid in water, 0.1%v/v: acetonitrile in gradient elution. Electrospray ionization (ESI) source was operated in the positive ion mode. Targeted MS/MS mode on a QTOF MS was used to quantify the drug utilizing the transitions of 340.1(m/z), 473.2 (m/z), 316.2 (m/z), 408.1 (m/z), and 357.1 (m/z) for ALO, LIN, SAX, SIT and PIO respectively. Results: As per ICH Q2R1 guidelines, a detailed validation of the method was carried out and the standard curves were found to be linear over the concentration ranges of 1516.0-4548.1 ng mL-1, 519.8- 1559.4 ng mL-1, 1531.4-4594.3 ng mL-1and 1519.6-4558.8 ng mL-1 for ALO, LIN, SAX and SIT respectively. Precision and accuracy results were within the acceptable limits. The mean recovery was found to be 98.8 _ 0.76 % (GEM), 102.2 _ 1.59 % (LIN), 95.3 _ 2.74 % (SAX) and 99.2 _ 1.75 % (SIT) respectively. Conclusions: The optimized validated UPLC QTOF-MS/MS method offered the advantage of shorter analytical times and higher sensitivity and selectivity. The optimized method is suitable for application in quantitative analysis of pharmaceutical dosage forms for QC laboratory.

scholarly journals Alanine Aminopeptidase, γ-Glutamyl Transferase and β2-microglobulin as Diagnostic Markers in Patients with Rheumatoid Arthritis

2008 ◽  
Vol 27 (1) ◽  
pp. 59-63
Author(s):  
Dejan Spasovski ◽  
Todor Gruev ◽  
Nada Marina ◽  
Jordan Calovski ◽  
Ljubinka Rajčevska ◽  
...  
Keyword(s):  
Rheumatoid Arthritis ◽  
Diagnostic Markers ◽  
Border Region ◽  
Healthy Individuals ◽  
Kinetic Assay ◽  
Renal Lesions ◽  
Alanine Aminopeptidase ◽  
Glutamyl Transferase ◽  
Higher Sensitivity

Alanine Aminopeptidase, γ-Glutamyl Transferase and β2-microglobulin as Diagnostic Markers in Patients with Rheumatoid Arthritis The purpose of this research is to evaluate the values of alanine aminopeptidase (AAP), γ-glutamyl transferase (γ-GT), and β2-Microglobulin in urine (β2-M), in untreated rheumatoid arthritis (RA) and to define the effect of untreated rheumatoid arthritis on the tubular function and brush border region. We used a kinetic assay for AAP, standard methods by the IFCC for γ-glutamyl transferase and MEIA for the determination of β2-Microglobulin in urine in 70 participants (35 untreated RA patients, 35 healthy individuals). From the total of 35 RA patients, 24 patients had AAP (sensitivity of the test 68.57%), 16 patients had γ-GT enzymuria (sensitivity of the test 45.71%), while the presence of β2-Microglobulin in urine was found in a very low percentage. Out of 18 RF negative patients, 14 patients are AAP positive, 10 patients were γ-GT positive, while the presence of β2-Microglobulin in urine was not detected. Among 17 RF positive RA patients, the presence of AAP was noticed in 10, the presence of γ-GT in 6 patients, while the presence of β2-Microglobulin in urine was not detected. AAP has higher sensitivity than γ-GT and β2-Microglobulin in the detection of asymptomatic renal lesions in untreated RA.

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