Colorimetric Determination of Arprinocid in Feed

1978 ◽  
Vol 61 (5) ◽  
pp. 1078-1082
Author(s):  
David W Fink ◽  
Kobert P Martin ◽  
James V Pivnichny ◽  
Jung-Sook K Shim

Abstract An analytical method has been developed for the determination of arprinocid (9-(2-chloro- fluorophenylmethyl) -9ff-purin-6-amine) in feed, based upon measurement of the absorbance of the diazo chromophore formed from product of zinc reduction of the drug in acidic solution. The analyte is extracted from the feed into chloroform in the presence of a pH 7 phosphate buffer and isolated by adsorption chromatography on alumina, followed by partitioning between hexane and 0.15M HC1. The reduction product in the aqueous phase is then treated for colorimetric measurement. This procedure has been applied to determining 0.0010-0.0080% arprinocid in feed with precision of <5% relative standard deviation near the middle of this concentration range. Of 32 feed additives examined, only zoalene and sulfamethazine were serious interferences. study and discussion of several factors, e.g., reaction time, pH, and amount of zinc metal, that affect the analytical reactions are also included.

1998 ◽  
Vol 52 (1) ◽  
pp. 101-105 ◽  
Author(s):  
L. F. Capitán-Vallvey ◽  
F. Ojeda ◽  
M. Del Olmo ◽  
R. Avidad ◽  
A. Navalón ◽  
...  

A method for nalidixic acid (NA) determination by transmitted room-temperature phosphorescence is proposed. The antibacterial agent NA in acidic solution shows native fluorescence; when NA is spotted on a filter paper precoated with β-cyclodextrin and lead (II) acetate and dried for 5 min, phosphorescence results. The transmitted phosphorescence was measured directly with the use of a homemade sample holder. The excitation and emission wavelengths were 330 and 417 nm, respectively. The applicable concentration range was between 0.06 and 4.50 μg/mL with a relative standard deviation of 2.8% and a detection limit of 0.02 μg/mL. The method was applied to the determination of NA in human urine and pharmaceuticals, with recoveries from 97.5 to 105.5%.


1994 ◽  
Vol 77 (6) ◽  
pp. 1557-1561 ◽  
Author(s):  
T Katrdna Pulliainen ◽  
Harriet C Wallin

Abstract A spectrophotometric method in which the sample is dry-ashed in the presence of zinc oxide, and total phosphorus content is measured colorimetrically as molybdenum blue was evaluated by 12 participating laboratories from the Nordic countries. The study included potato flour, sausage, cold ham, infant formula powder, cheese, and skimmed milk powder. The materials were presented to the participants as 12 randomly coded samples of 2 blind duplicates of each material. The phosphorus content of the materials varied between 0.076 and 0.96 g/100 g. The relative standard deviation for repeatability of the method varied from 1.1% for 0.96 g phosphorus/100 g to 5.4% for 0.29 g phosphorus/100 g. The relative standard deviation for reproducibility varied from 3.6% for 0.96 g phosphorus/100 g to 7.7% for 0.23 g phosphorus/100 g.


Author(s):  
Firas Hassan Awad

This paper aims to develop a simple, sensitive and accurate spectrophotometric method for quantitative determination of paracetamol in aqueous medium. The method is based on the reaction between the hydrolyzed paracetamol and 9-chloroacridine reagent (9-CA). The spectra of the product show maximum absorption at 436 nm. Beer's law is obeyed in the concentration range of 0.25-11 µg/mL with molar absorptivity value 5.3x103 L/mol/cm. The average recovery percentage (Rec%) is 99.27% and relative standard deviation (RSD) is :: 2.82%. In addition, the stability constant has been determined and the reaction mechanism is proposed. The method has been applied successfully for the assay of paracetamol in pharmaceutical formulations. It is found that the method does not require extraction process and it agree well with British pharmacopeia.    


2010 ◽  
Vol 3 (1) ◽  
pp. 9-13 ◽  
Author(s):  
Sophi Damayanti ◽  
Slamet Ibrahim ◽  
Kurnia Firman ◽  
Daryono H Tjahjono

Analytical method for the determination of paracetamol and ibuprofene mixtures has been developed by High Performance Liquid Chromatography using C-18 column and acetinitrile - phosphate buffer pH = 4.5 (75:25) containing 0.075% sodium hexanesulfunate as a mobile phase. The detector was set at 215 nm. Using such conditions, retention time for paracetamol and ibuprofen was 4.89 and 7.11 min, respectively. The recovery for paracetamol and ibuprofen was found to be 101.07± 0.73% and 102.02 ± 1.58%, respectively. The detector limits of the method was 1.30 and 1.60 μg/mL with the relative standard deviation (RSD) 0.74 and 1.52% for paracetamol and ibuprofen, respectively.   Keywords: paracetamol, ibuprofen, multi-component, validation, HPLC.


1969 ◽  
Vol 52 (1) ◽  
pp. 101-107
Author(s):  
C R Szalkowski ◽  
J Kanora

Abstract Ronidazole, (l-melhyl-5-nitroimidazoI- 2-yl)mcthyl carbamate, is extracted from finished poultry feeds with methanol and chromatographcd on an AL2O3-FIorex column. The eluate is concentrated and dissolved in CCI4 and the ronidazole is extracted with. H2O. The purified ronidazole is hydrolyzcd in NaOH solution in the presence of copper and p-aminobenzoic acid; the resulting diazonium compound is then coupled with naphthylethylenediamine to form a colored complex, which is measured spectrophotometrically at 550 mµ. No significant interference was found from finished feeds, domestic and foreign, or from 48 common feed additives. Recovery experiments on 36 laboratory-prepared feed samples at levels ranging from 0.0015 to 0.030% ronidazole averaged 100.8% with a standard deviation of 2.4.


2003 ◽  
Vol 86 (3) ◽  
pp. 476-483 ◽  
Author(s):  
Holly A Weber ◽  
Matthew K Zart ◽  
Andrew E Hodges ◽  
Kellie D White ◽  
Sarah M Barnes ◽  
...  

Abstract A fast, practical ambient extraction methodology followed by isocratic liquid chromatography (LC) analysis with UV detection was validated for the determination of berberine, hydrastine, and canadine in goldenseal (Hydrastis canadensis L.) root powder. The method was also validated for palmatine, a major alkaloid present in the possible bioadulterants Coptis, Oregon grape root, and bar-berry bark. Alkaloid standard solutions were linear over the evaluated concentration ranges. The analytical method was linear for alkaloid extraction using 0.3–2 g goldenseal root powder/100 mL extraction solvent. Precision of the method was demonstrated using 10 replicate extractions of 0.5 g goldenseal root powder, with percent relative standard deviation for all 4 alkaloids ≤1.6. Alkaloid recovery was determined by spiking each alkaloid into triplicate aliquots of neat goldenseal root powder. Recoveries ranged from 92.3% for palmatine to 101.9% for hydrastine. Ruggedness of the method was evaluated by performing multiple analyses of goldenseal root powder from 3 suppliers over a 2-year period. The method was also used to analyze Coptis root, Oregon grape root, barberry bark, and celandine herb, which are possible goldenseal bioadulterants. The resulting chromato-graphic profiles of the bioadulterants were significantly different from that of goldenseal. The method was directly transferred to LC with mass spectrometry, which was used to confirm the presence of goldenseal alkaloids tetrahydro-berberastine, berberastine, canadaline, berberine, hydrastine, and canadine, as well as alkaloids from the bioadulterants, including palmatine, jatrorrhizine, and coptisine.


Author(s):  
Hiroya Harino ◽  
Sayaka Midorikawa ◽  
Takaomi Arai ◽  
Madoka Ohji ◽  
Nguyen Duc Cu ◽  
...  

An analytical method for the simultaneous determination of five booster biocides (Sea-Nine 211, Dichlofluanid, Duiron, Irgarol 1051 and Pyrithiones) and degradation product of Irgarol 1051 (M1) in sediment from Vietnam was developed by LC/MS-MS. The recovery rates and relative standard deviation of the booster biocides in the sediment were in the range of 71–108% and 1.5–12%, respectively, and the detection limits were in the range of 0.04–2 μg kg−1 dry. An analytical method for the simultaneous determination of three booster biocides (Sea-Nine 211, Duiron and Irgarol 1051) and M1 in clams was also developed by LC/MS-MS. The recovery rates and relative standard deviations of the booster biocides in the biological samples were in the range of 60–99% and 3.4–6.8%, respectively, and the detection limits were in the range of 0.24–1.1 μg kg−1.The booster biocides in sediment from the coastal area of northern and central Vietnam were measured using this analytical method. Sea-Nine 211, Dichlofluanid, Duiron, Irgarol 1051, M1 and Pyrithiones were detected in the range of 0.09–1.3 μg kg−1 dry, <0.10–13 μg kg−1 dry, 0.11–3.0 μg kg−1 dry, 0.05–4.0 μg kg−1 dry, <0.1–0.43 μg kg−1 dry and <2–420 μg kg−1 dry, respectively. The detection frequencies of Dichlofluanid, M1 and Pyrithiones were low. The species and levels of detected booster biocides varied between sampling stations.Irgarol 1051 and its degradation product M1 were not detected in clams.


Author(s):  
Vikas Kumar Singh ◽  
Santosh Kumar Verma ◽  
Sudhanshu Ranjan Swain

A highly selective, specific, precise sensitive and reliable ICPMS method has been developed and validated by using ICP-MS for the determination of multielement in Sucroferric oxyhydroxide. The described ICP-MS method provides specific detection and quantification of minor and trace elements from 0.3J(30%) to 2J(200%) of its individual specification of each element i.e Ag, As, Au, Ba, Cd, Co, Cr, Cu, Hg, Ir, Li, Mo, Ni, Os, Pb, Pd, Pt, Rh, Ru, Sb, Se, Sn, Tl,  and V.The analytical method found to be Linear for each individual element with working concentration range from 30%, 50%, 100%, 150% and 200% i.e 0.3J, 0.5J, 1J, 1.5J and 2J with correlation coefficient not less than 0.990.The % recoveries of elemental impurities of each individual elements at three different concentrations with spiking in samples were found to be an acceptable range as 70% to 150%.The method was found to be precise and robust and its relative standard deviation was below 20%.The actual observed relative standard deviation in Precision was found to be in an acceptable range. Therefore developed method can be use for routine quantitative analysis of elemental impurities like Ag, As, Au, Ba, Cd, Co, Cr, Cu, Hg, Ir, Li, Mo, Ni, Os, Pb, Pd, Pt, Rh, Ru, Sb, Se, Sn, Tl, and V to ensure the quality of drug product.


Polymers ◽  
2021 ◽  
Vol 13 (17) ◽  
pp. 2847
Author(s):  
Furong Wang ◽  
Chao Du ◽  
Junjun Chen ◽  
Lisheng Shi ◽  
Hailong Li

The study aimed at developing a new spectrophotometric method for determining the pectin content. Take commercial pectin as an example, and the method is based on the reaction of copper ions with pectin to produce copper pectate. The spectrophotometer was used to measure the remaining content of copper ions so as to calculate the pectin content. This method eliminated the weight step and avoided the error associated with it. Effects of reaction time, temperature, and pH on absorbance were also studied. Additionally, the accuracy of this method was verified. It indicated excellent repeatability and accuracy with the relative standard deviation of 2.09%. In addition, three different plant types were used to demonstrate the reliability of the method. To summarize, this method can be widely used for the determination of pectin content in many materials.


Author(s):  
P.F. Collins ◽  
W.W. Lawrence ◽  
J.F. Williams

AbstractA procedure for the automated determination of ammonia in tobacco has been developed. Ammonia is extracted from the ground tobacco sample with water and is determined with a Technicon Auto Analyser system which employs separation of the ammonia through volatilization followed by colourimetry using the phenate-hypochlorite reaction. The procedure has been applied to a variety of tobaccos containing from 0.02 to 0.5 % ammonia with an overall relative standard deviation of 2 %. The accuracy of the procedure as judged by recovery tests and by comparison to a manual distillation method is considered adequate


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