Simplified Cleanup and Liquid Chromatographic Ultraviolet Determination of Linuron and Three Metabolites in Potatoes

1990 ◽  
Vol 73 (3) ◽  
pp. 435-437
Author(s):  
George E Miliadis ◽  
Panayotis A Siskos ◽  
George S Vasilikiotis
Keyword(s):  
Detection Limit ◽  
Field Experiment ◽  
Efficient Method ◽  
Mobile Phase ◽  
Uv Detection ◽  
Liquid Chromatographic

Abstract A simple and efficient method Is presented for the extraction, cleanup, and liquid chromatographic (LC) determination of linuron and 3 of Its metabolites, 3-(3,4-dlchlorophenyl)-1- methyl urea (DCPMU), 3-(3,4-dlchlorophenyl) urea (DCPU), and 3,4-dlchloroanillne (DCA), in potatoes. Samples are extracted with acetone, partitioned into dlchloromethanehexane (1 + 1), and cleaned up using disposable silica cartridges. LC determination Is performed using a LIChrosorb NH2 5 pm column, with an Isopropanol-lsooctane gradient mobile phase and UV detection at 248 nm. Recoveries of linuron and 2 of the metabolites from untreated samples fortified at 0.02-2 jtg/g ranged from 80 to 102%, while recoveries for the metabolite DCA ranged from 60 to 78%. The detection limit was 0.015 jtg/g for linuron and each metabolite; the minimum quantitation level was 0.5 fig/g. The developed method was applied to potato samples from a field experiment

Ultra-Performance Liquid Chromatographic and Densitometric Methods for Sensitive Determination of Xipamide and Triamterene in Pure and Pharmaceutical Dosage Forms

2021 ◽  
Author(s):  
N V Fares ◽  
Haitham A El Fiky ◽  
Amr M Badawey ◽  
Maha F Abd El Ghany
Keyword(s):  
Acetic Acid ◽  
Flow Rate ◽  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Uv Detection ◽  
Pharmaceutical Dosage Forms ◽  
Selective Determination ◽  
Liquid Chromatographic

Abstract Background Validated UPLC method and TLC densitometric method were prescribed for determination of antihypertensive components. Objectives: To establish and validate rapid and accurate Ultra performance liquid chromatographic (UPLC) and TLC densitometric methods for determination of Xipamide and Triamterene in pure and dosage forms. Methods The first method; UPLC method, depended on using Agilent Zorbax Eclipse Plus C8 (50 mm × 2.1 mm, 1.8 μm), as the column, mobile phase composed of (acetonitrile-water) (70 + 30, v/v) adjusted by acetic acid to obtain (pH 3), 0.2 mL/min flow rate and UV detection at 231.4 nm. The second method was a thin layer chromatography (TLC) densitometric method, separation was achieved by using toluene-methanol-ethyl chloride-acetic acid (7 + 2 + 1 + 0.2, v/v/v) as the mobile phase, pre coated silica gel plates as the stationary phase and UV detection at 300.0 nm. Results The obtained results were validated and statistically compared with official and reported methods. The obtained results showed high accuracy and reproducible results with excellent mean recoveries for both drugs. Conclusions The UPLC method showed shorter retention time for both Xipamide (0.88 min) and Triamterene (0.63 min), lower detection limit less than 0.055 µg/mL for both drugs with high selectivity, decreased injection volume (1 µL) and lower flow rate other than any HPLC method. Both proposed methods were sensitive, selective, and effectively applied to pure and dosage forms (Epitens®). Highlights Unprecedented sensitive, rapid, and reproducible UPLC and TLC methods were developed for selective determination of mixture of Xipamide and Triamterene with LOD less than 0.076 µg/mL for both drugs.

Determination of AmpiciUin and Amoxicillin in Milk with an Automated Liquid Chromatographic Cleanup

1994 ◽  
Vol 77 (1) ◽  
pp. 41-45 ◽  
Author(s):  
William A Moats
Keyword(s):  
Detection Limit ◽  
Sodium Dodecyl Sulfate ◽  
Mobile Phase ◽  
Chloride Solution ◽  
Sodium Dodecyl ◽  
Tetraethylammonium Chloride ◽  
Fraction Collector ◽  
Dodecyl Sulfate ◽  
Liquid Chromatographic

Abstract A method is described for determination of am-piciitin and amoxicillin in milk by using an automated liquid chromatographic (LC) cleanup. Milk was deproteinated by adding tetraethylammonium chloride solution and acetonitrile. The filtrate was concentrated by evaporation, filtered, and loaded into a 4 mL autosampler vial. For LC cleanup, a Waters W1SP 712 autosampler, a Varian 9010 pump, a Supelcosil LC-18 column, and an ISCO FOXY fraction collector were used. The cleanup program, where A is 0.01 M KH2PO4 and B is acetonitrile, was 100A + OB for 0-3 min and then 70A + 30B for 24 min. Sample concentrate (2 mL) was loaded onto the column for cleanup. Fractions containing amoxicillin and ampicillin were collected, partially acidified, and concentrated to 1 mL. Analysis was done on the LC-18 column, with a mobile phase of 0.015M H3PO4–{0.0075M sodium dodecyl sulfate-acetonitrile (70 + 30)] for amoxicillin and 0.0067M H3PO4–0.0033M KH2PO4–[0.005M sodium dodecyl sulfate–acetonitrile (67 + 33)] for ampicillin. Recoveries were generally 80–90% at a concentration range of 1–0.01 ppm, with a detection limit of 2–5 ppb. By collecting appropriate fractions, the method can be applied to the determination of any amphoteric β-lactam.

Simplified Cleanup and Liquid Chromatographic Determination of Oxamyl Residues in Potato Tubers

1985 ◽  
Vol 68 (4) ◽  
pp. 753-756
Author(s):  
Brian D Mcgarvey ◽  
Mikio Chiba ◽  
Theo H A Olthof
Keyword(s):  
Efficient Method ◽  
Mobile Phase ◽  
Chromatographic Determination ◽  
Size Exclusion ◽  
Minimum Detectable Concentration ◽  
Potato Tubers ◽  
Detectable Concentration ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simple and efficient method is presented for the extraction, cleanup, and liquid chromatographic (LC) determination of oxamyl residues in potato tubers. Samples are extracted with methanol, partitioned into dichloromethane, and cleaned up using Sep-Pak Florisil cartridges. LC determination is performed using a Zorbax PSM 60 size exclusion ; column with an acetonitrile-water (1 + 9) mobile phase and UV detection at 254 nm. Recovery of oxamyl from spiked control tubers averaged 94.1 and 85.9% at fortification levels of 0.4 and 0.08 \μg oxamyl/g tuber, respectively. The minimum detectable concentration of oxamyl by this method is 0.01 μg/g

A Green Liquid Chromatographic Method For The Simultaneous Determination of Chlorpheniramine Maleate, Pseudoephedrine Hydrochloride and Propyphenazone

2019 ◽  
Vol 15 (6) ◽  
pp. 635-641
Author(s):  
Nadia M. Mostafa ◽  
Ghada M. Elsayed ◽  
Nagiba Y. Hassan ◽  
Dina A. El Mously
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Dosage Form ◽  
Chromatographic Method ◽  
Green Analytical Chemistry ◽  
Chlorpheniramine Maleate ◽  
Accuracy And Precision ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Background:The concept of green analytical chemistry prevails due to the growing environmental pollution.Objective:Our attempts are to develop simple and eco-friendly method which is non-harmful to the environment by producing minimal waste. In this context, a green liquid chromatographic method was applied for the simultaneous determination of chlorpheniramine maleate, pseudoephedrine hydrochloride and propyphenazone in their combined dosage form.Methods:Separation was carried out using X select HSS RP C18 analytical column (250 × 4.6 mm, 5μm) using methanol - 0.02 M phosphate buffer pH 3 - triethylamine (60:40: 0.1, by volume) as a mobile phase. The separated peaks were detected at 215 nm at a flow rate 1.0 mL/min.Results:Quantification was done over the concentration ranges of 1-25 µg/mL for chlorpheniramine maleate, 5-35 µg/mL for pseudoephedrine hydrochloride and 10-120 µg/mL for propyphenazone. The suggested method was validated with regard to linearity, accuracy and precision according to the International Conference on Harmonization guidelines with good results.Conclusion:It could be used as a safer alternative for routine analysis of the mentioned drugs in quality control laboratories.

Liquid Chromatographic Determination of Sulfamoyldapsone in Swine Tissues

1987 ◽  
Vol 70 (6) ◽  
pp. 1031-1032
Author(s):  
Yuuko S Endoh ◽  
Ryozo Yamaoka ◽  
Nobuo Sasaki
Keyword(s):  
Detection Limit ◽  
Quantitative Determination ◽  
Chromatographic Determination ◽  
Alumina Column ◽  
Average Recovery ◽  
Diaminodiphenyl Sulfone ◽  
Alumina Column Chromatography ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method is described for the quantitative determination of sulfamoyldapsone (2-sulfamoyl-4,4'-diaminodiphenyl sulfone) in swine muscle, liver, kidney, and fat. Sulfamoyldapsone was extracted from tissues with acetonitrile saturated with n-hexane. The extract was washed with n-hexane saturated with acetonitrile, concentrated, and cleaned up by alumina column chromatography. Sulfamoyldapsone was separated on an ODS column by using acetonitrile-methanol-water (6 + 18 + 76) and was detected at 292 nm. Overall average recovery of sulfamoyldapsone added to tissues at levels of 0.1 and 0.5 /μg/g was 93.3% ± 6.0. Detection limit was 0.02 μg/g in these tissues.

scholarly journals QUANTIFICATION OF BILASTINE AND MONTELUKAST COMBINATION IN FORMULATIONS UTILIZING LIQUID CHROMATOGRAPHY: STABILITY STUDIES

2021 ◽  
pp. 210-215
Author(s):  
KANCHARLA VIJAYALAKSHMI ◽  
BETHAPUDI SAMUEL ANAND ANDREWS ◽  
BOLINENI NAGESWARA RAO
Keyword(s):  
Liquid Chromatography ◽  
Detection Limit ◽  
Mobile Phase ◽  
Tablet Formulation ◽  
Uv Detection ◽  
Stability Studies ◽  
Stability Indicating ◽  
Quantitation Limit ◽  
Rp Hplc

Objective: We have developed a “stability-indicating RP-HPLC” procedure for the Bilastine (BLS) and montelukast (MTL) analysis of tablets. Methods: The quantification of BLS and MTL combination was implemented utilising a Waters column (C18, 5 μm, 250 mm and 4.6 mm). Isocratic mobile phase had 60% volume KH2PO4 of 0.1M strength with pH 4.2 units and 40% volume methanol at a flow with 1.0 ml/min speed. UV detection at 232 nm was done to examine BLS and MTL. Stability experiments of BLS and MTL under distinctive environments of stress were also performed. Results: The BLS and MTL were eluted at 1.810 min and 2.551 min, respectively. The responses were found to be linear for the concentration ranges of 10-30 µg/ml (BLS) and 5-15 µg/ml (MTL). Percent comparative standard deviance for precision was 0.331% (BLS) and 0.486% (MTL). Percent assay for accuracy was 98.96% (BLS) and 99.00% (MTL). The detection limit and quantitation limit measures for BLS were 0.018 µg/ml and 0.059 µg/ml, respectively, while for MTL it was 0.024 µg/ml and 0.081 µg/ml, respectively. Robustness studies authorized that the method is robust with percent comparative standard deviance of a highest 1.950%. Conclusion: The developed “stability-indicating RP-HPLC” procedure for the BLS and MTL analysis is simple, sensitive, precise, specific and robust, making it appropriate to the assessment of BLS and MTL in a tablet formulation.

Improved liquid-chromatographic determination of haloperidol in plasma.

1984 ◽  
Vol 30 (7) ◽  
pp. 1228-1230 ◽  
Author(s):  
A K Dhar ◽  
H Kutt
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Room Temperature ◽  
Internal Standard ◽  
Isoamyl Alcohol ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract This method for determination of haloperidol in plasma is based on "high-performance" isocratic liquid chromatography with the use of a C8 bonded reversed-phase column at room temperature. Haloperidol and the internal standard (chloro-substituted analog) are extracted from alkalinized plasma into isoamyl alcohol/heptane (1.5/98.5 by vol) and back-extracted into dilute H2SO4. The aqueous phase is directly injected onto the column. The mobile phase is a 30/45/25 (by vol) mixture of phosphate buffer (16.5 mmol/L, pH 7.0), acetonitrile, and methanol. Unlike other liquid-chromatographic procedures for haloperidol, commonly used psychotropic drugs do not interfere. Analysis can be completed within an hour. The procedure is extremely sensitive (1.0 microgram/L) and is well reproducible (CV 5.6% for a 2.5 micrograms/L concentration in plasma).

Spectrofluorometric Determination of BAY Vp 2674 Residues in Poultry Tissues

1987 ◽  
Vol 70 (5) ◽  
pp. 813-818 ◽  
Author(s):  
T Bill Waggoner ◽  
Malcolm C Bowman
Keyword(s):  
Detection Limit ◽  
Fluorescence Detection ◽  
Coefficient Of Variation ◽  
Organic Extract ◽  
Spectrofluorometric Determination ◽  
Poultry Tissues ◽  
Liquid Chromatographic

Abstract A spectrofluorometric (SPF) method is described for determination of residues of BAY Vp 2674 in chicken and turkey tissues. The drug is extracted from tissues with dichloromethane-methanol. The organic extract is concentrated to near dryness and cleaned up by a series of partitionings with n-hexane, then dichloromethane against pH 2 buffer and dichloromethane against pH 12 buffer. The drug is partitioned into dichloromethane from pH 7 buffer and concentrated to dryness. The residue is dissolved in pH 3.5 buffer for SPF analysis at 282 nm (excitation) and 445 nm (emission). Recoveries of BAY Vp 2674 added to chicken and turkey tissues at levels of 0.05, 0.1, and 0.2 ppm range from 86 to 92% with a coefficient of variation of 3.4-10.1%. Detection limit is 0.02 ppm. A liquid chromatographic confirmatory procedure is also described, with ultraviolet and fluorescence detection

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