Influence of reagent purity on the ion chromatographic determination of bromate in water using 3,3′-dimethoxybenzidine as a prochromophore for photometric detection

2000 ◽  
Vol 2 (6) ◽  
pp. 571-575 ◽  
Author(s):  
Edward T. Urbansky ◽  
Stephanie K. Brown
1985 ◽  
Vol 68 (3) ◽  
pp. 545-546
Author(s):  
Michael Tsougros

Abstract A stability indicating liquid chromatographic method for the determination of diazepam in tablets was collaboratively studied by 6 laboratories. The method uses a Cig reverse phase column, a methanolwater mobile phase, p-tolualdehyde as the internal standard, and photometric detection at 254 nm. The collaborators were supplied with a synthetic tablet powder and 3 commercial tablet samples. The mean recovery of diazepam from the synthetic tablet powder was 100.2%. For all samples analyzed, the coefficient of variation was < 1.5%. The method has been adopted official first action.


1984 ◽  
Vol 67 (2) ◽  
pp. 339-341
Author(s):  
David J Krieger

Abstract A simple, rapid LC method is presented for the separation and determination of acetaminophen in analgesic preparations containing up to 6 additional active components. The method uses a C18 reverse phase column, methanol–0.75% acetic acid (1 + 3) mobile phase, and photometric detection in the ultraviolet region. Acetaminophen was effectively separated from chlorpheniramine maleate, phenylephrine hydrochloride, caffeine, salicylamide, aspirin, and phenacetin, as well as from salicylic acid, a degradation product of aspirin. Typical chromatograms of the separation of acetaminophen from the above compounds in synthetic mixture and in commercial multicomponent analgesic preparations are presented, along with reproducibility and recovery data.


1987 ◽  
Vol 70 (5) ◽  
pp. 834-836
Author(s):  
Ella S Moore

Abstract A liquid chromatographic method for the determination of coumarin anticoagulants in tablets was collaboratively studied by 7 laboratories. The method uses an octadecylsilane-bonded microparticulate column, tetrahydrofuran-methanol-water-acetic acid mobile phase, and photometric detection at 311 nm. Each collaborator received samples of warfarin sodium, phenprocoumon, and dicumarol as a synthetic composite and as commercial individual and composited tablets. Pooled average assay values for synthetic and commercial tablet samples of warfarin sodium were 101.6 and 99.5%, respectively, with a combined reproducibility SD of 2.38% (CV = 2.37%) and combined repeatability SD of 1.49% (CV = 1.49%). Pooled average (SD) assay values for dicumarol and phenprocoumon commercial samples were 98.0 (2.27) and 101.3% (4.00), respectively. The content uniformity determinations of 2 mg warfarin sodium and 25 mg dicumarol tablets indicated average tablet contents (range) of 99.5% (91.0-116.0) and 98.0% (89.8-108.8), respectively. The method has been approved interim official first action


1997 ◽  
Vol 80 (3) ◽  
pp. 549-554 ◽  
Author(s):  
Karl-Erik Hellenás ◽  
Carina Branzell ◽  
H Poutanen ◽  
T Suortti ◽  
R Kaario ◽  
...  

Abstract Twelve laboratories participated in a collaborative study to evaluate precision parameters of a liquid chromatographic method for analysis of the glycoalkaloids α-solanine and α-chaconine in potato tubers. Samples consisted of frozen potato tuber homogenates distributed as 3 blind duplicates and 3 split-level pairs. The analytical method included aqueous extraction, workup on disposable solidphase extraction cartridges, and reversed-phase chromatography with photometric detection at 202 nm. Results for α-solanine and α-chaconine were received from 10 and 9 laboratories, respectively. Relative standard deviations for reproducibilo ity for α-solanine and α-chaconine were similar, ranging from 8 to 13% in the applied concentration range of 12 to 260 mg/kg fresh weight.


1991 ◽  
Vol 585 (2) ◽  
pp. 315-317 ◽  
Author(s):  
Atsushi Yamamoto ◽  
Akinobu Matsunaga ◽  
Eiichi Mizukami ◽  
Kazuichi Hayakawa ◽  
Motoichi Miyazaki

1992 ◽  
Vol 75 (3) ◽  
pp. 511-518 ◽  
Author(s):  
Valerio Leoni ◽  
Anna M Caricchia ◽  
Salvatore Chiavarini

Abstract A critical review of multiresidue analytical methods was performed to develop an easy procedure that can be applied with slight modifications to vegetable and animal food samples. The multiresidue method described Is applicable to the quantitative determination of 28 organophosphorus pesticides In fatty as well as nonfatty foods. The foods are divided Into 4 groups according to extraction process (acetone and acetone-water for samples with moisture content <45%) and cleanup (on active carbon- Cellte, on disposable mlnicolumns of Kieselguhr- type material, and on disposable mlnicolumns of bonded-phase silica, according to fat and pigment content). A further fractionation on silica-gel microcolumns can be Included In the procedure. A wide-bore column (SPB-5) with flame photometric detection operated in phosphorus mode (FPD-P) was chosen for gas chromatographic determination. Recoveries from apples, olive oil, whole milk, pasta, and eggs are reported. Two packed columns (4% OV-101 and SP2250- SP2401) with FPD-P were tested as confirmation columns. The method is suitable for a total diet study.


1983 ◽  
Vol 66 (5) ◽  
pp. 1196-1202
Author(s):  
Samuel T Walker ◽  
◽  
R Balbach ◽  
E Jefferson ◽  
D Jordan ◽  
...  

Abstract A previously reported high pressure liquid chromatographic method for the determination of amitriptyline hydrochloride in dosage forms was modified to permit its use as a stability-indicating method. The modified method, entailing a nitrile bonded microparticulate column, a methanol-0.005M ammonium acetate (90 + 10) mobile phase, and photometric detection at 239 nm, was collaboratively tested by 10 laboratories. Each collaborator received samples of synthetic and commercial tablets and injections. The recovery from a synthetic injection at the 10.06 mg/mL spiking level averaged 98.6%. The amount of declared found in commercial injections averaged 103.1%. The pooled reproducibility SD (CV%) and repeatability SD (CV%) were ± 2.12 (2.15) and ± 1.81 (1.84), respectively. The recovery from synthetic tablet composite at the 7.45% spiking level averaged 102.0%. The amount of declared found for commercial 25 mg and 100 mg tablets averaged 96.7 and 97.9%, respectively. The pooled reproducibility SD (CV%) and repeatability SD (CV%) for these 3 tablet samples were ± 1.89 (1.86) and ± 1.66 (1.64), respectively. Content uniformity analysis of commercial 25 mg and 100 mg tablets (n = 10) gave amounts of declared values averaging 100.5% (range 92.4-108.8%) and 99.3% (range 89.6-107.0%), respectively. The pooled reproducibility SD (CV%) and repeatability SD (CV%) were ± 3.23 (3.2) and ± 2.78 (2.8), respectively. A commercial injectable preparation spiked with dibenzosuberone was also collaboratively analyzed by a thin layer method. The method was adopted interim official first action.


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