Determination of Reserpine in Tablets by Liquid Chromatography with Fluorescence Detection: Revised Procedure

1994 ◽  
Vol 77 (3) ◽  
pp. 758-760
Author(s):  
Ugo R Cieri
Keyword(s):  
Aqueous Solution ◽  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Sodium Salt ◽  
Filter Paper ◽  
Mobile Phase ◽  
Small Volume ◽  
Slight Modification ◽  
Reference Solution

Abstract A procedure is presented for the determination of reserpine in tablets by liquid chromatography (LC) that is a slight modification of a method presented in a previous publication. The sample is extracted with methanol, and solutions are filtered through filter paper. For LC, a 7.5 cm column is used; the mobile phase is methanol containing a small volume of an aqueous solution of the sodium salt of 1-pentanesulfonic acid. Detection is by fluorescence with 280 nm excitation and 360 nm emission. Two commercial samples containing 0.1 and 0.25 mg reserpine were analyzed. For each sample, 2 determinations were made on a ground composite. Ten tablets were also analyzed individually. A linearity study was conducted, with solutions ranging in concentration from 80 to 120% of the amount present in the reference solution.

Determination of Ajmalicine in Reserpine Raw Materials by Liquid Chromatography with Fluorescence Detection

1995 ◽  
Vol 78 (4) ◽  
pp. 944-945 ◽  
Author(s):  
Ugo R Cieri
Keyword(s):  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Mobile Phase ◽  
Small Volume ◽  
Raw Materials ◽  
Normal Phase ◽  
Reference Solution ◽  
Acid Sodium Salt ◽  
Phase Column

Abstract A method is presented for determination of ajmalicine in reserpine raw materials by liquid chromatography (LC) with fluorescence detection. The sample is dissolved in a very small volume of chloroform, and the resulting solution is diluted with methanol. The reference solution of ajmalicine is prepared directly in methanol. For LC, a 30 cm long normal-phase column is used. The mobile phase is methanol containing a small volume of an aqueous solution of 1-pentanesulfonic acid, sodium salt. Detection is by fluorescence with excitation at 280 nm and emission at 360 nm. In 3 samples, the ajmalicine contents ranged from 1.2 to 1.9%.

scholarly journals Multiresidue Determination of Fluoroquinolones in Eggs

2000 ◽  
Vol 83 (6) ◽  
pp. 1306-1312 ◽  
Author(s):  
Marilyn J Schneider ◽  
Dan J Donoghue
Keyword(s):  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Small Volume ◽  
Reversed Phase ◽  
Reversed Phase Liquid Chromatography ◽  
Trace Enrichment ◽  
On Line ◽  
Phase Liquid ◽  
Multiresidue Determination

Abstract A multiresidue method was developed for the determination of fluoroquinolones in eggs. Extraction of eggs with ammoniacal acetonitrile was followed by liquid–liquid defatting, solvent evaporation, and redissolution in a small volume of buffer. The fluoroquinolones were further purified by on-line microdialysis, concentrated on a trace enrichment column, and separated by reversed-phase liquid chromatography with fluorescence detection. Norfloxacin (NOR), ciprofloxacin (CIP), and sarafloxacin (SAR) were extracted from fortified eggs over a range of 2–200 μg/kg, with recoveries of 65.7–78.9%, 65.6–77.1%, and 67.6–110%, respectively. Enrofloxacin (ENRO) was extracted over a range of 1–100 μg/kg, with recoveries of 71.5–86.7%, whereas desethylene ciprofloxacin (DCIP) and danofloxacin (DANO) were extracted over a range of 0.2–20 μg/kg, with recoveries of 68.7–90.7% and 76.0–93.8%, respectively. The limits of quantitation for the 6 fluoroquinolones were as follows: DCIP and DANO, 0.3 μg/kg; ENRO, 1 μg/kg; NOR and CIP, 2 μg/kg; and SAR, 3 μg/kg. Both SAR and ENRO incurred eggs were also successfully analyzed using this method.

scholarly journals Rapid Determination of Nosiheptide in Meat and Egg by Liquid Chromatography with Fluorescence Detection

2000 ◽  
Vol 83 (1) ◽  
pp. 17-19 ◽  
Author(s):  
Shozo Horii ◽  
Naoto Oku
Keyword(s):  
Liquid Chromatography ◽  
Phosphoric Acid ◽  
Fluorescence Detection ◽  
Mobile Phase ◽  
Lower Layer ◽  
Rapid Determination ◽  
Chicken Muscle

Abstract A procedure was developed to determine nosiheptide residues in marketed meat and egg. Acetonitrile was used for the extraction, and the extract was partitioned with hexane to remove fat. The lower layer was reconstructed and quantitated by liquid chromatography using fluorescence detection at 357 nm excitation and 500 nm emission. The mobile phase consisted of 0.025% phosphoric acid–acetonitrile (50 + 50, v/v). Recoveries of nosiheptide from fortified samples ranged from 91.3 to 95.2% for swine muscle, 88.6 to 92.7% for chicken muscle, and 86.3 to 86.8% for egg. The method was used to monitor swine and chicken muscle and egg (20 samples each) in the market. Nosiheptide was not determined in all 60 samples.

Determination of Small Quantities of Atropine in Commercial Preparations by Liquid Chromatography with Fluorescence Detection

1985 ◽  
Vol 68 (5) ◽  
pp. 1042-1045
Author(s):  
Ugo R Cieri
Keyword(s):  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Small Volume ◽  
Steam Bath ◽  
Atropine Sulfate ◽  
Excitation Wavelength ◽  
Fluorescence Detector ◽  
Commercial Sample ◽  
Relative Standard

Abstract A method is presented for the determination of small quantities of atropine in commercial preparations by liquid chromatography (LC) with fluorescence detection. The sample is extracted with CHC13 from basic suspension, the CHC13 is evaporated on the steam bath, and the dry residue is dissolved in a small volume of CH3OH. A reverse phase column is used for the LC analysis; the eluting solvent is prepared by mixing 950 mL CH3OH with 50 mL water containing 1 g of the sodium salt of l-pentanesulfonic acid. The fluorescence detector is set at an excitation wavelength of 255 nm and an emission wavelength of 285 nm. Several commercial tablets and injections containing atropine in combination with other ingredients and a commercial sample of belladonna extract were analyzed by the proposed method. Recoveries of atropine sulfate from aqueous solutions averaged 100.7% with a relative standard deviation (RSD) of 3.35% for atropine sulfate levels of 0.12 mg. Recoveries of atropine sulfate from synthetic injection formulations were 99.8 and 100.0% withRSDsof 2.03and2.35%, respectively; the atropine sulfate concentrations of commercial injections with the same formulations were found to be 97.0 and 100.0% of the labeled amounts with RSDs of 0.53 and 1.46%, respectively

Application of Silica Nanoparticles in the Determination of Herbicides in Environmental Water Samples Using Liquid Chromatography-Mass Spectroscopy

2020 ◽  
Vol 16 (5) ◽  
pp. 748-756
Author(s):  
Mir Waqas Alam ◽  
Tentu Nageswara Rao ◽  
Yarasani Prashanthi ◽  
Vourse Sridhar ◽  
Adil Alshoaibi ◽  
...  
Keyword(s):  
Aqueous Solution ◽  
Liquid Chromatography ◽  
Silica Nanoparticles ◽  
Solid Phase ◽  
Silica Nanoparticle ◽  
Environmental Water ◽  
Phase Extraction ◽  
Functionalized Nanoparticles ◽  
Supporting Material

Background: Herbicides are very beneficial in the crop yield with the aid of controlling weeds within the agriculture, but several herbicides are chronic in soil. Objective: In this study, nanoparticles and the packages of synthesized novel silica nanoparticles were studied for the preconcentration of herbicides. Methods: These nanoparticles prepared by the Stöber mechanism were purified and functionalized. Nanoparticles thus prepared successfully were used as supporting material for the preconcentration of residues of herbicides in the water. Results: Preconcentration was achieved by preparing the silica-based solid-phase-extraction cartridges. Nanoparticles used for this purpose were within the range of 50-250 nm. An SPE cartridge was prepared by packing 200 mg of silica nanoparticle in the empty cartridge of diameter 5.5 cm and length 0.6 cm in between PTFE frits. Aqueous solutions of 0.1 μg/ml of herbicides were prepared separately, and 10 ml of the solution was passed through the cartridge at the rate of 0.2 ml/min. After passing 10 ml volume of the aqueous solution, residues adsorbed on the cartridge were eluted using 2 ml of acetonitrile. The eluate was injected to determine the herbicide residue adsorbed on the SPE cartridge. Conclusion: In the study, it was found that greater than 90% of the herbicide residues were trapped on silica nanoparticle-based SPE cartridge. An analytical method was developed for the simultaneous determination of these herbicides. The residues were quantified by LC-MS/MS with ESI mode.

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