Detection of trace amounts of abamectin used as an antiparasitic agent in fallow deer tissues

2009 ◽  
Vol 57 (1) ◽  
pp. 99-107 ◽  
Author(s):  
Diana Žele ◽  
Silvestra Kobal ◽  
Gorazd Vengušt ◽  
Andrej Bidovec ◽  
Anton Vengušt ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Fallow Deer ◽  
Reversed Phase ◽  
Fat Tissue ◽  
Matrix Interference ◽  
Solid Phase Extraction Cartridge ◽  
Tissue Matrix

A sensitive and reliable method for the determination of trace amounts of abamectin in muscles, kidneys and fat tissue of fallow deer is presented. Abamectin was extracted from the tissues with acetonitrile and the extract was cleaned up on a C8 solid-phase extraction cartridge. Abamectin residue was derivatised with trifluoroacetic acid anhydride and 1-methylimidazole, and determined using reversed- phase high-performance liquid chromatography under isocratic conditions and fluorescence detection. The recoveries of the method were high and consistent, ranging from 78% to 90%. The limit of detection of the method was below 1 μg/kg when analysing muscle, kidney and fat tissue. Matrix-matched calibration was used in order to obtain accurate values and to avoid matrix interference.

scholarly journals Detection and Quantitative Estimation of Toxic Acrylamide Levels in Selected Potatoes Chips and French Fries from the Libyan Market Using HPLC-UV Method

2021 ◽  
Vol 36 (2) ◽  
pp. 106-115
Author(s):  
Osama I. G. Khreit ◽  
Abdulsalam Elfowiris ◽  
Abdulrahman A. Aljali ◽  
Omukalthum Abduljalil
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Quantitative Estimation ◽  
Reversed Phase ◽  
French Fries ◽  
Detector Response ◽  
Limit Of Quantification ◽  
Potential Health

Acrylamide is a potential health hazardous compound occurring in baked and fried food as a result of excessive dry heating during the preparation and/or processing of foods. Exposure to a high level of acrylamide may cause cancer, neurotoxicity, and mutagenicity. In this study, an isocratic reversed-phase high-performance liquid chromatographic (HPLC) method using a C18 column was used for the determination of acrylamide in selected food. The mobile phase consisted of 0.1% formic acid in water: acetonitrile (98:02), and the flow rate was 1.0 mL min-1, elution was monitored at 200 nm. Validation in selected conditions showed that the chosen method is sensitive, selective, precise, and reproducible with a linear detector response for the determination of acrylamide. The limit of detection (LOD), and the limit of quantification (LOQ), were achieved at 0.41μg mL-1 and 1.25 μg mL-1respectively. The proposed method was also applied after validation to the most popular six brands of chips and French fries available in the Libyan market. Acrylamide was extracted by a simplified extraction method avoiding cleanup by solid-phase extraction (SPE), then analyzed by HPLC-UV. The highest level of acrylamide was found in one brand of chips with a concentration of 16.33 μg mL-1, whereas only one of the French fries products analyzed exhibited an acrylamide concentration of 10.26 μg mL-1.

Determination of tigecycline in turkey plasma by LC-MS/MS: validation and application in a pharmacokinetic study

2017 ◽  
Vol 20 (2) ◽  
pp. 241-249 ◽  
Author(s):  
A. Jasiecka-Mikołajczyk ◽  
J.J. Jaroszewski
Keyword(s):  
Pharmacokinetic Study ◽  
High Performance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Reversed Phase ◽  
Selected Reaction Monitoring ◽  
Limit Of Quantification ◽  
Complicated Skin ◽  
Intravenous And Oral Administration

Abstract Tigecycline (TIG), a novel glycylcycline antibiotic, plays an important role in the management of complicated skin and intra-abdominal infections. The available data lack any description of a method for determination of TIG in avian plasma. In our study, a selective, accurate and reversed-phase high performance liquid chromatography-tandem mass spectrometry method was developed for the determination of TIG in turkey plasma. Sample preparation was based on protein precipitation and liquid-liquid extraction using 1,2-dichloroethane. Chromatographic separation of TIG and minocycline (internal standard, IS) was achieved on an Atlantis T3 column (150 mm × 3.0 mm, 3.0 μm) using gradient elution. The selected reaction monitoring transitions were performed at 293.60 m/z → 257.10 m/z for TIG and 458.00 m/z → 441.20 m/z for IS. The developed method was validated in terms of specificity, selectivity, linearity, lowest limit of quantification, limit of detection, precision, accuracy, matrix effect, carry-over effect, extraction recovery and stability. All parameters of the method submitted to validation met the acceptance criteria. The assay was linear over the concentration range of 0.01-100 μg/ml. This validated method was successfully applied to a TIG pharmacokinetic study in turkey after intravenous and oral administration at a dose of 10 mg/kg at various time-points.

Detection, Quantitation, and Identification of Residual Aminopenicillins by High-Performance Liquid Chromatography after Fluorescamine Derivation

2000 ◽  
Vol 63 (10) ◽  
pp. 1421-1425 ◽  
Author(s):  
CHIH-CHUN HONG ◽  
FUSAO KONDO
Keyword(s):  
Bovine Serum ◽  
Mobile Phase ◽  
High Performance ◽  
Serum Proteins ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Excitation Wavelength ◽  
Column Temperature ◽  
Solid Phase Extraction Cartridge ◽  
Mobile Phases

A high-performance liquid chromatographic (HPLC) method with fluorescence detection after precolumn fluorescamine derivation was developed to detect residues of two aminopenicillins, amoxicillin (AMPC) and ampicillin (ABPC), in bovine serum. Proteins in serum samples spiked with each of these penicillins were precipitated with sodium tungstate and sulfuric acid, centrifuged, and removed by passage through a C18 solid-phase extraction cartridge. After precolumn treatment of the extraction products of AMPC and ABPC with fluorescamine solution, HPLC analysis with fluorescence spectrophotometric detection at an excitation wavelength of 390 nm and an emission wavelength of 485 nm was performed to identify these products. Two mobile phases were used for residual analysis by the isocratic HPLC system. An ODP column (polyvinyl alcohol bonded with an octadecyl functional group) that can be used with strongly alkaline mobile phases (pH 2.0 to 13) was selected, and the column temperature was set at 40°C. A mobile phase comprising 100-mM K2HPO4 solution and acetonitrile (72:28, vol/vol), which yielded AMPC and ABPC retention times of 4.1 and 7.9 min, respectively, was suitable for detection of residual ABPC but not for residual AMPC because interference was caused by peaks of other extracted substances. When a mobile phase comprising a different ratio of 100-mM K2HPO4 solution and acetonitrile (78:22, vol/vol) was used, the retention times of AMPC and ABPC were 7.3 and 26.3 min, respectively, and both penicillins could be analyzed using this system. The calculated standard curves of the reaction products with both mobile phases were linear, and the correlation coefficients were greater than 0.999. The lower limit of detection was 10 ng/ml for both penicillins. Analysis of extracts from bovine serum spiked with AMPC and ABPC at a concentration of 1 μg/ml yielded recovery rates of 102.2 ± 5.5% and 79.0 ± 5.2%, respectively. This detection method may be useful for routine laboratory testing of AMPC and ABPC.

scholarly journals Development and validation of reversed phase high performance liquid chromatography (RP-HPLC) for quantification of captopril in rabbit plasma

2020 ◽  
Author(s):  
Muhammad Fawad Rasool ◽  
Umbreen Fatima Qureshi ◽  
Nazar Muhammad Ranjha ◽  
Imran Imran ◽  
Mouqadus Un Nisa ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Rabbit Plasma ◽  
Rp Hplc ◽  
Relative Standard

AbstractTh accurate rapid, simple and selective reversed phase high performance liquid chromatography (RP-HPLC) has been established and validated for the determination of captopril (CAP). Chromatographic separation was accomplished using prepacked ODSI C18 column (250 mm × 4.6 mm with 5 μm particle size) in isocratic mode, with mobile phase consisting of water: acetonitrile (60:40 v/v), pH adjusted to 2.5 by using 85% orthophosphoric acid at a flow rate of 1 mL/min and UV detection was performed at 203 nm. RP-HPLC method used for the analysis of CAP in mobile phase and rabbit plasma was established and validated as per ICH-guidelines. It was carried out on a well-defined chromatographic peak of CAP was established with a retention time of 4.9 min and tailing factor of 1.871. The liquid–liquid extraction method was used for extraction of CAP from the plasma. Excellent linearity (R2 = 0.999) was shown over range 3.125–100 µg/mL with mean percentage recoveries ranges from 97 to 100.6%. Parameters of precision and accuracy of the developed method meet the established criteria. Intra and inter-day precision (% relative standard deviation) study was also performed which was less than 2% which indicate good reproducibility of the method. The limit of detection (LOD) and quantification for the CAP in plasma were 3.10 and 9.13 ng/mL respectively. The method was suitably validated and successfully applied to the determination of CAP in rabbit plasma samples.

scholarly journals RP-HPLC analysis for the simultaneous estimation of rabeprazole sodium and aceclofenac in a combined dosage form

2012 ◽  
Vol 1 (12) ◽  
pp. 410-413 ◽  
Author(s):  
Sukhbir Lal Khokra ◽  
Balram Choudhary ◽  
Heena Mehta
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Pharmaceutical Journal ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Simultaneous Estimation ◽  
Rp Hplc ◽  
Rabeprazole Sodium

A rapid, simple and highly sensitive reversed phase high performance liquid chromatographic (RP-HPLC) method has been developed for the quantitative determination of Rabeprazole sodium and Aceclofenac in a combined dosage form. Rabeprazole sodium and Aceclofenac were chromatographed using C-18 column as stationary phase and methanol: acetonitrile: water (60 : 10 : 30 v/v/v) as the mobile phase at a flow rate of 1.0 ml/min at ambient temperature and detected at 280 nm. The retention time (RT) of Rabeprazole sodium and Aceclofenac were found to be 5.611 min and 2.102 minute, respectively. The linearities of Rabeprazole sodium and Aceclofenac were in the range of 1-10 µg/ml and 3-15 µg/ml, respectively. The limit of detection was found to be 0.091 µg/ml for Rabeprazole sodium and 0.043 µg/ml for Aceclofenac. The proposed method was applied for the determination of Rabeprazole sodium and Aceclofenac in a combined dosage form and result was found satisfactory.DOI: http://dx.doi.org/10.3329/icpj.v1i12.12450 International Current Pharmaceutical Journal 2012, 1(12): 410-413

scholarly journals Determination of Flumorph Residues in Vegetables, Soil, and Natural Water by Solid-Phase Extraction Cleanup and High-Performance Liquid Chromatography with UV Detection

2008 ◽  
Vol 91 (6) ◽  
pp. 1459-1466 ◽  
Author(s):  
Ji-Ye Hu ◽  
Yu-Chao Zhang ◽  
Hai Yan
Keyword(s):  
Solid Phase Extraction ◽  
Natural Water ◽  
High Performance ◽  
Solid Phase ◽  
Residue Analysis ◽  
Reversed Phase ◽  
Uv Detection ◽  
Phase Extraction ◽  
Limit Of Quantification

Abstract A method for high-performance liquid chromatographic (HPLC) determination of flumorph residues in cucumber, tomato, soil, and natural water was developed and validated. Primary secondary amine or octadecylsilyl (C18) solid-phase extraction cartridges were used for sample preparation. Reversed-phase HPLC with UV detection was used for separation and quantification of the pesticide. The combined cleanup and chromatographic method steps were sensitive and reliable for simultaneous determination of residues of the 2 isomers of flumorph in the studied samples. This method is characterized by recovery >97.9, coefficient of variation <6.2, and limit of quantification of 0.01 mg/kg, in agreement with directives for method validation in residue analysis. Flumorph residues in the samples were further confirmed by HPLC/mass spectrometry. The proposed method is fast, easy to perform, and could be used for monitoring of pesticide residues.

scholarly journals Determination of Vitamin K1 in Medical Foods by Liquid Chromatography with Postcolumn Reduction and Fluorometric Detection

2000 ◽  
Vol 83 (4) ◽  
pp. 957-962 ◽  
Author(s):  
George M Ware ◽  
G William Chase ◽  
Ronald R Eitenmiller ◽  
Austin R Long
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Sodium Bicarbonate Solution ◽  
Reversed Phase ◽  
Mean Value ◽  
Fluorometric Detection ◽  
Vitamin K1 ◽  
Limit Of Quantitation ◽  
Medical Foods

Abstract A liquid chromatographic (LC) method is described for the determination of vitamin K1 in medical foods. The sample is enzymatically digested with lipase and α-amylase and extracted with 1% sodium bicarbonate solution–isopropanol (1 + 1). After C18 solid-phase extraction, vitamin K1 is separated by nonaqueous reversed-phase LC, converted to the hydroquinone by postcolumn zinc reduction, and quantitated by fluorescence detection. The limit of detection is 8 pg (3 σ), and the limit of quantitation is 27 pg (10 σ) on column. Linear response ranged from 0.1 to 1.0 ng vitamin K1 (r = 0.9999). The mean recovery (n = 38) for all spiking levels was 101.6 ± 2.85%. Analysis of Standard Reference Material 1846, Infant Formula, gave a mean value of 0.95 ± 0.088 mg vitamin K/kg (K or K1?)(n = 31) with a coefficient of variation of 9.26.

Determination of Mimosine and 2,3-Dihydroxypyridine in Leucaena leucocephala by Reversed Phase High-Performance Liquid Chromatography

2011 ◽  
Vol 140 ◽  
pp. 296-301 ◽  
Author(s):  
Cai Mei Wu ◽  
Hong Min Yuan ◽  
Gang Jia ◽  
Zhi Sheng Wang ◽  
Xiu Qun Wu
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Leucaena Leucocephala ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Quantitative Detection ◽  
Uv Detector ◽  
Chromatography Method

A reversed high performance liquid chromatography method was developed for the quantitative determination of mimosine and 2,3-DHP in leaves ofLeucaena Leucocephala. Mimosine and 2,3DHP were extracted using 0.1N HCl.The chromatograph conditions were investigated and optimized. The optimal HPLC conditions as follows: Agilent HC-C18 column （4.6×150mm,5μm） was used at 30°C. The method used a variable wavelength UV detector at 280nm, the mobile phase consisted of 0.2 % (w/v) orthophosphoric acid and methanol, the gradient elution was adopted. The injection volume was 10μL. The linearity is favorable in the range of 1.0 to 50μg mL-1with a correlation coefficient of 0.99998 for mimosine and 0.99902 for 2,3DHP. Under the optimal conditions, the method limit of detection (LOD) of mimosine and 2,3DHP were 0.40mg/kg and 0.55mg/kg respectively. The recovery of mimosine was 87.00-94.70% with the RSD (n=5) of 2.75-3.81% in the spiked levels 0,1, 5, 20mg/g. At the same time, the recovery of 2,3DHP was 88-95.4% with the RSD (n=5) of 2.24-4.90%. The method was found to be simple, sensitive, fast and accurate, and has been applied successfully for the quantitative detection of mimosine and 2,3-DHP in leaves ofLeucaena Leucocephala, plasma and excretion of ruminant.

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