Simultaneous Liquid Chromatographic Determination of Fenamiphos and Its Metabolites in Soil

1992 ◽  
Vol 75 (1) ◽  
pp. 62-65 ◽  
Author(s):  
R Khazanchi ◽  
S Walia ◽  
S K Handa
Keyword(s):  
Chromatographic Method ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A reversed-phase liquid chromatographic method has been developed for the determination of fenamiphos and the metabolites fenamiphos sulfoxide, fenamiphos sulfone, 3-methyl-4-(methylthlo)- phenol, and 3-methyl-4-(methylsulflnyl)phenol. Trace quantities of the nematlclde and Its metabolites In soil can be determined simultaneously. The limit of detection of the method was 5 ppm. Recoveries of fenamiphos and Its degradation products at fortification levels of 25,50, and 100 ppm ranged from 99.2 to 100.8%. Standard deviations ranged from 0.29 to 0.70 ppm.

Gas-Liquid Chromatographic Determination of T-2 Toxin in Plasma

1983 ◽  
Vol 66 (4) ◽  
pp. 909-912 ◽  
Author(s):  
Steven P Swanson ◽  
Venkatachalam Ramaswamy ◽  
Val R Beasley ◽  
William B Buck ◽  
Harold H Burmeister
Keyword(s):  
Chromatographic Method ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Aqueous Sodium Hydroxide ◽  
Chromatographic Determination ◽  
Florisil Column ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract The gas-liquid chromatographic method for the determination of T-2 toxin in plasma is described. The toxin is extracted with benzene, washed with aqueous sodium hydroxide, and chromatographed on a small Florisil column; the heptafluorobutyryl derivative is prepared by reaction with heptafluorobutyrylimidazole. The T-2 HFB derivative is chromatographed onOV-1 at 230°C and measured with an electron capture detector. Iso-T-2, an isomer of T-2 toxin, is added to samples as an internal standard before extraction. Recoveries averaged 98.0 ± 5.5% at levels ranging from 50 to 1000 ng/m L. The limit of detection is 25 ng/mL.

Liquid Chromatographic Determination of Thiamine in Rodent Feed by Postcolumn Derivatization and Fluorescence Detection

1995 ◽  
Vol 78 (2) ◽  
pp. 307-309 ◽  
Author(s):  
Theresa A Gehring ◽  
Willie M Cooper ◽  
Claude L Holder ◽  
Harold C Thompson
Keyword(s):  
Chromatographic Determination ◽  
Reversed Phase ◽  
Detector Response ◽  
Fluorescence Excitation ◽  
Liquid Chromatographic Method ◽  
Essential Nutrient ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method was developed for determination of the essential nutrient thiamine (vitamin Bi) in rodent feed. Thiamine was extracted with hydrochloric acid, separated by reversed-phase liquid chromatography, derivatized postcolumn to thiochrome with potassium hydroxide and potassium ferricyanide, and detected by fluorescence. Excitation and emission wavelengths were 370 and 430 nm, respectively. Detector response was linear in the range of 2.58 to 15.5 ng of thiamine injected. Instrument detection limit was 5 pg of thiamine injected.

Liquid Chromatographic Determination of Aflatoxin M1 in Milk Powder Using Immunoaffinity Columns for Cleanup: Interlaboratory Study

1993 ◽  
Vol 76 (6) ◽  
pp. 1248-1254 ◽  
Author(s):  
Louis G M Th Tuinstra ◽  
Arie H Roos ◽  
John M P Van Trijp ◽  
◽  
P A Burdaspal ◽  
...  
Keyword(s):  
Milk Powder ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Interlaboratory Study ◽  
Aflatoxin M1 ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method for determining low aflatoxin M1 concentrations in milk was evaluated in an International Dairy Federation (IDF) interlaboratory study. The study involved 16 participants from 11 countries. The method, chosen after a comparison of several methods by a preparatory group, uses an immunoaffinity column for cleanup. As the sample passes through the column, antibodies selectively bind with aflatoxin M1 (antigen) present and form an antibody-antigen complex. All other components of the sample matrix are washed off the column with water. Then, aflatoxin M1 is eluted from the column with acetonitrile, which is collected. Final determination is carried out by reversed-phase liquid chromatography with fluorescence detection. Over the tested range (80-600 ng aflatoxin M1/kg milk powder), an RSDR ranging from 11 to 23% was obtained by analyzing 24 samples (blind duplicates), 2 samples of which were blanks.

Reversed-Phase Liquid Chromatographic Determination of Cromolyn Sodium in Drug Substance and Select Dosage Forms

1994 ◽  
Vol 77 (6) ◽  
pp. 1689-1694 ◽  
Author(s):  
Linda L Ng
Keyword(s):  
Technical Communication ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Liquid Chromatographic Method ◽  
Validation Parameters ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract This study, presented as a technical communication, describes a reversed-phase liquid chromatographic method for select commercial formulations, namely, inhalation solution, nasal solution, capsule and inhalation aerosol. Miscellaneous validation parameters are also discussed.

Liquid Chromatographic Determination of Methyldopa and Methyldopa-Thiazide Combinations in Tablets: Collaborative Study

1984 ◽  
Vol 67 (6) ◽  
pp. 1118-1120
Author(s):  
Ting Susan ◽  
◽  
R L Brown ◽  
L A Dougherty ◽  
J B Schepman ◽  
...  
Keyword(s):  
Chromatographic Method ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Repeatability And Reproducibility ◽  
Liquid Chromatographic

Abstract A reverse phase liquid chromatographic method for the determination of methyldopa, methyldopa-hydrochlorothiazide, and methyldopachlorothiazide in tablets was collaboratively studied by 8 laboratories. Each collaborator received 20 samples that included drug substance, synthetic and commercial tablet compositions. The overall repeatability and reproducibility standard deviations for commercial tablets were 1.11 and 1.75% for methyldopa, 0.96 and 1.62% for chlorothiazide, and 1.21 and 2.15% for hydrochlorothiazide, respectively. The overall recoveries of methyldopa, chlorothiazide, and hydrochlorothiazide added to synthetic tablets were 100.78, 100.70, and 101.34%, respectively. The method has been adopted official first action.

Liquid Chromatographic Determination of Medroxyprogesterone Acetate in Tablets

1988 ◽  
Vol 71 (3) ◽  
pp. 528-530 ◽  
Author(s):  
Aqeel A Fatmi ◽  
Gregory V Williams ◽  
Elizabeth A Hickson
Keyword(s):  
Medroxyprogesterone Acetate ◽  
Chromatographic Method ◽  
Ammonium Phosphate ◽  
Chromatographic Determination ◽  
Photometric Detection ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A reverse-phase liquid chromatographic method is described for the assay of medroxyprogesterone acetate in tablets. An octadecylsilane (C18) column with a mobile phase of methanol-O.OlM dibasic ammonium phosphate (80 + 20 v/v, pH 7.2 ± 0.1) and photometric detection at 254 nm separates medroxyprogesterone acetate from excipients. Detector responses were linear to concentrations of medroxyprogesterone acetate over the range 50-150 μg/mL (r = 0.999). Mean recovery of medroxyprogesterone acetate added to tablet excipients was 100.8%. Mean assay results were 101.3% (n = 3). The assay results are comparable to those obtained by the compendial liquid chromatographic method

scholarly journals Reversed-Phase Liquid Chromatographic Determination of Two Manufacturing Intermediates in D&C Red No. 34 and Its Lakes

2009 ◽  
Vol 92 (6) ◽  
pp. 1639-1643 ◽  
Author(s):  
Bhakti Petigara Harp ◽  
Julie N Barrows
Keyword(s):  
Chromatographic Method ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Lower Accuracy ◽  
Naphthoic Acid ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic ◽  
Column Chromatographic

Abstract A reversed-phase LC method was developed to determine two manufacturing intermediates in the monosulfo monoazo color additive D&C Red No. 34 and its lakes. The analytes are 2-amino-1-naphthalenesulfonic acid (Tobias acid) and 3-hydroxy-2-naphthalenecarboxylic acid (3-hydroxy-2-naphthoic acid). This method can be used for batch certification of the color additives by the U.S. Food and Drug Administration to ensure that each lot meets published specifications for coloring drugs and cosmetics. The new method uses lithium oxalate in methanolwater to dissolve the color additives for analysis. The analytes were identified by comparison of their LC retention times and UV absorption spectra with those of standards. Peak area calibrations were generally linear (R > 0.999) and recoveries were 105 for Tobias acid and 103 for 3-hydroxy-2-naphthoic acid. The limits of determination (LOD) were 0.01 for Tobias acid and 0.03 for 3-hydroxy-2-naphthoic acid. The RSDs at the specification levels were 0.9 for Tobias acid and 3.2 for 3-hydroxy-2-naphthoic acid. Survey analyses of 14 samples of certified D&C Red No. 34 straight colors and lakes from six domestic and foreign manufacturers yielded results for Tobias acid that generally agreed with results previously obtained by using a gravity elution column chromatographic method. Nine of the results for 3-hydroxy-2-naphthoic acid were 2 to 5 times higher than the results obtained using the column chromatographic method. We attribute the lower accuracy of the column chromatographic method to incomplete solubility of the samples using the method conditions and difficulty with interpreting the UV spectrophotometric results.

scholarly journals Determination of Cefdinir by a Stability-Indicating Liquid Chromatographic Method

2005 ◽  
Vol 88 (6) ◽  
pp. 1661-1665 ◽  
Author(s):  
Tushar N Mehta ◽  
Gunta Subbaiah ◽  
Kilambi Pundarikakshudu
Keyword(s):  
Chromatographic Method ◽  
Degradation Products ◽  
Reversed Phase ◽  
Stability Indicating ◽  
Pharmaceutical Ingredients ◽  
Degraded Samples ◽  
Liquid Chromatographic Method ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A simple, fast, specific, stability-indicating, and precise reversed-phase liquid chromatographic method was developed for the determination of Cefdinir in its different dosage forms, i.e., capsules and suspensions. The method was developed and optimized by analyzing the placebo preparation, formulations, and degraded samples of the drug substance according to the International Conference on Harmonization. The proposed method can successfully separate the drug from degradation products formed under stress conditions along with pharmaceutical ingredients such as preservatives. The developed method was used successfully to determine Cefdinir in capsules and Insta-use suspensions. The developed method was found to be linear for a concentration range of 6–14 μg/mL. Average recoveries obtained with the method were 99.3 ± 0.4 and 99.6 ± 0.4% for Insta-use suspensions and capsules, respectively. The method was shown to be specific, precise, and robust.

scholarly journals Validated Reversed-Phase Liquid Chromatographic Method with Gradient Elution for Simultaneous Determination of the Antiviral Agents: Sofosbuvir, Ledipasvir, Daclatasvir, and Simeprevir in Their Dosage Forms

Molecules ◽  
2020 ◽  
Vol 25 (20) ◽  
pp. 4611
Author(s):  
Essam Ezzeldin ◽  
Nisreen F. Abo-Talib ◽  
Marwa H. Tammam ◽  
Yousif A. Asiri ◽  
Abd El-Galil E. Amr ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Chromatographic Method ◽  
Limit Of Detection ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Liquid Chromatographic Method ◽  
Phase Liquid ◽  
Liquid Chromatographic

A simple, rapid, sensitive, and precise reversed-phase liquid chromatographic method was developed and validated for the simultaneous determination of four direct-acting antivirals, sofosbuvir (SF), ledipasvir (LD), declatasvir (DC), and simeprevir (SM), in their respective pharmaceutical formulations. Effective chromatographic separation was achieved on an Agilent Eclipse plus C8 column (250 mm × 4.6 mm, 5 µm) at 40 °C with gradient elution using a mobile phase composed of acetonitrile:phosphate buffer (pH 6.5). The quantification of SF and DC was based on peak area measurements at 260 nm, while the quantification of LD and SM was achieved at 330 nm. The linearity was acceptable from 1.0 to 20.0 μg/mL for the studied drugs, with correlation coefficients >0.999. The analytical performance of the newly proposed HPLC procedure was thoroughly validated according to ICH guidelines in terms of linearity, precision (RSD%, 0.39–1.57), accuracy (98.05–101.90%), specificity, limit of detection (LOD) (0.022–0.039 μg/mL), limit of quantification (LOQ) (0.067–0.118 μg/mL), and robustness. The validated HPLC method was successfully used to analyze the abovementioned drugs in their pure and dosage forms without interference from common excipients present in commercial formulations.

scholarly journals Liquid Chromatographic Determination of Nystatin in Pharmaceutical Preparations

2001 ◽  
Vol 84 (4) ◽  
pp. 1050-1056 ◽  
Author(s):  
Phyllis Wilson ◽  
Ann Stewart ◽  
Valerie Flournoy ◽  
S William Zito ◽  
Ales Vancura
Keyword(s):  
Pharmaceutical Preparations ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Liquid Chromatographic Method ◽  
Peak Areas ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Bulk Drug ◽  
Liquid Chromatographic

Abstract A rapid, reversed-phase liquid chromatographic method was developed for the assay of nystatin in the bulk drug and a variety of dosage forms. Analysis was performed on a Symmetry C18 reversed-phase column using a mobile phase of methanol–water–dimethylformamide (DMF; 55 + 30 + 15, v/v/v), with detection by UV at 305 nm. Quantitation is based on the sum of the peak areas of the 2 major isomers of nystatin. The linearity of the assay was determined for a concentration range of 0.05 to 0.2 mg/mL (correlation coefficient > 0.999). Accuracies and precision showed good reproducibility.

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