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

Determination of the Malachite Green in Sediment by High Performance Liquid Chromatography with Fluorescence Detection

2013 ◽  
Vol 781-784 ◽  
pp. 942-946 ◽  
Author(s):  
Jian Chao Deng ◽  
Xian Qing Yang ◽  
Lai Hao Li ◽  
Jian Wei Cen ◽  
Shu Xian Hao ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Malachite Green ◽  
Fluorescence Detection ◽  
High Performance ◽  
Solid Phase ◽  
Fluorescence Detector ◽  
Sediment Samples ◽  
Relative Standard

A new method of determination of malachite green (MG) in sediment has been developed by high performance liquid chromatography with fluorescence detection (HPLC-FLD). It is based on use of a deoxidation reaction which converts malachite green (MG) into LMG in the process of extraction. The sediment samples were extracted with a solution of formic acid and acetonitrile. Clean up and isolation was performed on MCX solid phase extraction (SPE) column. Chromatographic separation was achieved by using C18column with an isocratic mobile phase consisting of acetonitrile and ammonium acetate buffer (0.05 M, pH 4.5) (80:20, v/v). High performance liquid chromatography with fluorescence detector (λex=265 nm and λem=360 nm) was used for the determination of LMG. The recovery values of MG in sediment samples fortified with MG were determined by measuring the amount of MG in the samples, after carrying out deoxidation reaction with potassium borohydride, which converts the MG into LMG. Under the optimized conditions, the average recoveries of MG from sediment at three levels (1.0, 10 and 50 μg/kg) were 85.0% (range from 80.8 to 87.6%). Relative standard deviations (RSD) of recoveries at all fortification levels were less than for 9.57% for MG. The method detection limit obtained for MG was 0.5 μg/kg.

Development and Validation of a New Method for the Determination of Anti-hepatitis C Agent Simeprevir in Human Plasma using HPLC with Fluorescence Detection

2020 ◽  
Vol 16 (4) ◽  
pp. 428-435
Author(s):  
Ahmed F.A. Youssef ◽  
Yousry M. Issa ◽  
Kareem M. Nabil
Keyword(s):  
Hepatitis C ◽  
Human Plasma ◽  
Fluorescence Detection ◽  
Internal Standard ◽  
Protein Precipitation ◽  
Assay Method ◽  
Fluorescence Detector ◽  
Limit Of Quantification ◽  
Relative Standard

Background: Simeprevir is one of the recently discovered drugs for treating hepatitis C which is one of the major diseases across the globe. Objective: The present study involves the development of a new and unique High-Performance Liquid Chromatography (HPLC) method using fluorescence detection for the determination of simeprevir (SIM) in human plasma. Methods: Two methods of extractions were tested, protein precipitation using acetonitrile and liquidliquid extraction. A 25 mM dipotassium hydrogen orthophosphate (pH 7.0)/ACN (50/50; v/v), was used as mobile phase and C18 reversed phase column as the stationary phase. The chromatographic conditions were optimized and the concentration of simeprevir was determined by using the fluorescence detector. Cyclobenzaprine was used as an internal standard. Results: Recovery of the assay method based on protein precipitation was up to 100%. Intra-day and inter-day accuracies range from 92.30 to 107.80%, with Relative Standard Deviation (RSD) range 1.65-8.02%. The present method was successfully applied to a pharmacokinetic study where SIM was administered as a single dose of 150 mg SIM/capsule (Olysio®) to healthy individuals. Conclusion: This method exhibits high sensitivity with a low limit of quantification 10 ng mL-1, good selectivity using fluorescence detection, wide linear application range 10-3000 ng mL-1, good recovery and highly precise and validation results. The developed method can be applied in routine analysis for real samples.

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.

Determination of Total Taurine in Pet Foods by Liquid Chromatography of the Dansyl Derivative: Collaborative Study

2000 ◽  
Vol 83 (4) ◽  
pp. 784-788 ◽  
Author(s):  
Kieran McCarthy ◽  
Claudia Hischenhuber ◽  
Neil Joyce ◽  
G Cherix ◽  
C Hischenhuber ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Collaborative Study ◽  
Gradient Elution ◽  
Taurine Concentration ◽  
Dansyl Derivative ◽  
Relative Standard ◽  
Standard Deviations ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method for the determination of total taurine in pet foods was evaluated in a collaborative study. Ten laboratories assayed 6 blind duplicate pairs of wet and dry pet foods. The taurine in the 6 sample pairs ranged from low (170 mg/kg) to high (2250 mg/kg) concentrations as is. Collaborators also assayed a sample of known taurine concentration for familiarization purposes. Samples were hydrolyzed to release bound taurine, which was subsequently converted to the dansyl derivative and quantitated by gradient-elution LC with fluorescence detection. Repeatability relative standard deviations, RSDr, ranged from 3.2 to 10.0%; reproducibility relative standard deviations, RSDR, ranged from 6.1 to 16.1%. The method has been adopted Official First Action status by AOAC INTERNATIONAL.

scholarly journals Multiresidue Determination of Fluoroquinolones in Shrimp by Liquid Chromatography-Fluorescence-Mass Spectrometryn

2005 ◽  
Vol 88 (4) ◽  
pp. 1160-1166 ◽  
Author(s):  
Marilyn J Schneider ◽  
Luz Vazquez-Moreno ◽  
Maria del Carmen Bermudez-Almada ◽  
Ramon Barraza Guardado ◽  
Magdalena Ortega-Nieblas
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
Phosphate Buffer ◽  
Fluorescence Detector ◽  
Relative Standard ◽  
Product Ions ◽  
Multiresidue Determination ◽  
Shrimp Tissue

Abstract An efficient multiresidue method for analysis of fluoroquinolones in shrimp has been developed in which quantitation by fluorescence and confirmation by Multiple Stage Mass Spectrometry (MSn) is achieved simultaneously. In this method, shrimp tissue is extracted with ammoniacal acetonitrile and the extract is defatted and then evaporated. After dissolution in basic phosphate buffer, fluoroquinolones in the extract are separated by liquid chromatography and quantitated, taking advantage of their intense fluorescence. Eluate from the fluorescence detector enters the MSn, which allows for confirmation by monitoring ratios of 2 prominent product ions in the MS3 or MS2 spectrum. Using this method, 8 fluoroquinolones have been analyzed in shrimp samples fortified at 10, 25, 50, or 100 ppb levels. Recoveries for desethyleneciprofloxacin, norfloxacin, ciprofloxacin, danofloxacin, enrofloxacin, orbifloxacin, sarafloxacin, and difloxacin ranged from 75 to 92%, with relative standard deviation values of <6%. The limits of quantitation ranged from 0.1 to 1 ng/g. Enrofloxacin and ciprofloxacin were also successfully determined in enrofloxacin-incurred shrimp using this method.

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.

scholarly journals Determination of Flumequine in Channel Catfish by Liquid Chromatography with Fluorescence Detection

1999 ◽  
Vol 82 (3) ◽  
pp. 614-619 ◽  
Author(s):  
Steven M Plakas ◽  
Kathleen R El Said ◽  
F Aladar Bencsath ◽  
Steven M Musser ◽  
Calvin C Walker
Keyword(s):  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Ictalurus Punctatus ◽  
Channel Catfish ◽  
Solid Phase ◽  
Signal To Noise Ratio ◽  
Methanol Solution ◽  
Signal To Noise ◽  
Relative Standard

Abstract Rapid methods are described for determination of flumequine (FLU) residues in muscle and plasma of farm-raised channel catfish (Ictalurus punctatus). FLU residues were extracted from tissues with an acidified methanol solution, and extracts were cleaned up on C18 solid-phase extraction cartridges. FLU concentrations were determined by liquid chromatography (LC)using a C18 analytical column and fluorescence detection (excitation, 325 nm; emission, 360 nm). Mean recoveries of FLU from fortified muscle were 87–94% at 5 levels ranging from 10 to 160 ppb (5 replicates per level). FLU recoveries from fortified plasma were 92–97% at 5 levels ranging from 20 to 320 ppb. Limits of detection (signal-to-noise ratio, 3:1)for the method as described were 3 and 6 ppb for muscle and plasma, respectively. Relative standard deviations (RSDs) for recoveries were ≤12%. Live catfish were dosed with 14C-labeled or unlabeled FLU to generate incurred residues. Recoveries of 14C residues throughout extraction and cleanup were 90 and 94% for muscle and plasma, respectively. RSDs for incurred FLU at 2 levels in muscle and plasma ranged from 2 to 6%. The identity of FLU in incurred tissues was confirmed by LC/mass spectrometry.

Determination of Zearalenone in Corn by High Pressure Liquid Chromatography and Fluorescence Detection

1978 ◽  
Vol 61 (5) ◽  
pp. 1058-1062
Author(s):  
George M Ware ◽  
Charles W Thorpe
Keyword(s):  
High Pressure ◽  
Liquid Chromatography ◽  
High Pressure Liquid Chromatography ◽  
Fluorescence Detection ◽  
Hplc Analysis ◽  
Fluorescence Detector ◽  
Reverse Phase

Abstract A method is reported for determining zearalenone in corn at levels as low as 10 ng/g. Samples are extracted with chloroform-water and cleaned up by liquid-liquid chromatography, and the zearalenone is detected by a fluorescence detector after separation by reverse phase high pressure liquid chromatography (HPLC). Recoveries of zearalenone added to corn at levels from 10 to 200 ng/g averaged greater than 89%. In addition, a confirmation procedure is described which involves sequential HPLC analysis of the sample and a zearalenone standard, using 4 different excitation wavelengths and comparing fluorescence responses obtained. This method was successfully applied to the analysis of 11 samples of cornmeal; zearalenone was detected in 9 of the samples at levels from 11 to 69 ng/g.

scholarly journals Simultaneous Determination of Albendazole and Its Three Metabolites in Pig and Poultry Muscle by Ultrahigh-Performance Liquid Chromatography-Fluorescence Detection

Foods ◽  
2021 ◽  
Vol 10 (10) ◽  
pp. 2350
Author(s):  
Zhaoyuan He ◽  
Zhixiang Diao ◽  
Yawen Guo ◽  
Kaizhou Xie ◽  
Lan Chen ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Solid Phase ◽  
Liquid Liquid Extraction ◽  
Hydrophilic Lipophilic Balance ◽  
Relative Standard ◽  
Albendazole Sulfone ◽  
Ultrahigh Performance Liquid Chromatography ◽  
Acquity Uplc

A fast, simple and efficient ultrahigh-performance liquid chromatography-fluorescence detection (UPLC-FLD) method for the determination of residues of albendazole (ABZ) and its three metabolites, albendazole sulfone (ABZ-SO2), albendazole sulfoxide (ABZ-SO), and albendazole-2-aminosulfone (ABZ-2NH2-SO2), in pig and poultry muscle (chicken, duck and goose) was established. The samples were extracted with ethyl acetate, and the extracts were further subjected to cleanup by utilizing a series of liquid–liquid extraction (LLE) steps. Then, extracts were purified by OASIS® PRiME hydrophilic-lipophilic balance (HLB) solid-phase extraction (SPE) cartridges (60 mg/3 mL). The target compounds were separated on an ACQUITY UPLC® BEH C18 (2.1 mm × 100 mm, 1.7 μm) chromatographic column, using a mobile phase composed of 31% acetonitrile and 69% aqueous solution (containing 0.2% formic acid and 0.05% triethylamine). The limits of detection (LODs) and limits of quantification (LOQs) of the four target compounds in pig and poultry muscle were 0.2–3.8 µg/kg and 1.0–10.9 µg/kg, respectively. The recoveries were all above 80.37% when the muscle samples were spiked with the four target compounds at the LOQ, 0.5 maximum residue limit (MRL), 1.0 MRL, and 2.0 MRL levels. The intraday relative standard deviations (RSDs) were less than 5.11%, and the interday RSDs were less than 6.29%.

scholarly journals Simultaneous determination of the residues of fourteen quinolones and fluoroquinolones in fish samples using liquid chromatography with photometric and fluorescence detection

2012 ◽  
Vol 30 (No. 1) ◽  
pp. 74-82 ◽  
Author(s):  
F. Cañada-Cañada ◽  
A. Espinosa-Mansilla ◽  
A. Jiménez Girón ◽  
A. Muñoz de la Peña
Keyword(s):  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Excitation Wavelength ◽  
Diode Array ◽  
Pipemidic Acid ◽  
Citrate Buffer ◽  
Fish Samples ◽  
Wavelength Emission ◽  
Uv Visible

A chromatographic method is described for assaying fourteen quinolones and fluoroquinolones (pipemidic acid, marbofloxacin, norfloxacin, ciprofloxacin, danofloxacin, lomefloxacin, enrofloxacin, sarafloxacin, difloxacin, oxolinic acid, nalidixic acid, flumequine, and pyromidic acid) in fish samples. The samples were extracted with m-phosphoric acid/acetonitrile mixture (75:25, v/v), purified, and preconcentrated on ENV + Isolute cartridges. The determination was achieved by liquid chromatography using C<sub>18</sub> analytical column. A mobile phase composed of mixtures of methanol-acetonitrile-10mM citrate buffer at pH 4.5, delivered under optimum gradient program, at a flow rate of 1.5 ml/min, allows accomplishing the chromatographic separation in 26 minutes. For the detection were used serial UV-visible diode-array at 280 nm and 254 nm and fluorescence detection at excitation wavelength/emission wavelength: 280/450, 280/495, and 280/405 nm. The detection and quantification limits were between 0.2–9.5and 0.7–32 µg/kg, respectively. The procedure was applied to the analysis of spiked salmon samples at two different concentration levels (50 µg/k and 100 µg/kg). Mean recoveries of fluoroquinolones from the salmon samples ranged from 50% to 102%, depending on the analyte.  

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