scholarly journals Liquid Chromatographic Determination of α-Solasonine in Frozen Green Peas as an Indicator of the Presence of Nightshade Berries

2003 ◽  
Vol 86 (4) ◽  
pp. 759-763 ◽  
Author(s):  
Peter Cavlovic ◽  
Mohan Mankotia ◽  
Peter Pantazopoulos ◽  
Peter M Scott
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Solanum Nigrum ◽  
Expanded Uncertainty ◽  
Method Performance ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Green Peas

Abstract Nightshade berries containing glycoalkaloids can be a contaminant in green peas. Methodology was developed to detect this contamination. The glycoalkaloid α-solasonine was extracted from frozen green peas with 1% (v/v) acetic acid, cleaned up on a C18 cartridge, and determined by liquid chromatography with UV detection at 200 nm. Method performance characteristics for the determination of α-solasonine include linearity from 140 to 1500 ng injected (r = 0.9996–0.9999); recovery ranging from 68 to 79%; limit of quantitation (LOQ) = 4.5 ppm (280 ng standard), and limit of detection = 0.64 ppm (40 ng standard). At the LOQ, the expanded uncertainty at 95% confidence was 0.38 × the reported value. The method was applied to the detection of α-solasonine in frozen green peas in a 2-year study of 60 samples of frozen green peas from Ontario, Canada. None of the samples contained α-solasonine. No unripe berries of Solanum nigrum were detected visually in the samples.

Liquid Chromatographic Determination of 5-(Methylamino)-2-Phenyl-4-[3-(Trifluoromethyl)phenyl]-3-(2H)-Furanone in Soil

1990 ◽  
Vol 73 (2) ◽  
pp. 298-299
Author(s):  
Thomas C Mueller ◽  
Philip A Banks ◽  
Parshall B Bush ◽  
William C Steen
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Soil Samples ◽  
Soil Types ◽  
Liquid Chromatographic Separation ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A rapid, sensitive method is described for the determination of5-(methylamlno)-2-phenyl-4-[3-(trlfluoromethyl)phenyl]-3- (2M)-furanone (RE-40885) concentrations in 3 soil types. The method consists of extraction of soil samples with methanol, filtration, liquid chromatographic separation of methanolsoluble components using a C18 column, and UV detection at 275 nm. Recoveries were 94, 96, and 94% from the Greenville, Cecil, and Dothan soils, respectively. Average relative standard deviation was 8.0% in the Greenville soil. The qualitative limit of detection was 20 ppb and the limit of quantitation was 40 ppb in 25 g soil samples.

scholarly journals Liquid Chromatographic Determination of Nicarbazin in Feeds

2000 ◽  
Vol 83 (5) ◽  
pp. 1027-1038 ◽  
Author(s):  
Beverly J Krabel ◽  
David A Dickson ◽  
Alan G Zimmermann ◽  
Mark R Coleman
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Linear Range ◽  
Limit Of Quantitation ◽  
Standard Linear ◽  
Sample Recovery ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A new liquid chromatographic method has been developed for determination of nicarbazin in feeds. Approximately 40 g feed is extracted with 200 mL acetonitrile–water (80 + 20, v/v). An aliquot of the extract is filtered and assayed using a reversed-phase isocratic method that measures the 4,4′–dinitrocarbanilide moiety of nicarbazin at a wavelength of 340 nm. For medicated feeds, the method uses a standard linear range of 5 to 100 μg/mL. For lower levels, a linear range of 50 to 150 ng/mL can be used. The method has a limit of detection of 250 ng/g and a limit of quantitation of 500 ng/g in a 40 g feed sample. Recovery was 99.1%, with a range of 95.2 to 101.8%. In the typical U.S. dosing range of 27 to 113.5 g/ton, the precision of the method based on one analyst, one day, and 2 weighings ranged from 2.8% (113.5 g/ton) to 4.7% (27 g/ton).

Liquid Chromatographic Determination of Amiodarone Hydrochloride and Related Compounds in Raw Materials and Tablets

1994 ◽  
Vol 77 (6) ◽  
pp. 1447-1453 ◽  
Author(s):  
Pauline M Lacrok ◽  
Norman M Curran ◽  
Wing-Wah Sy ◽  
Dennis K J Goreck ◽  
Pierre Thibault ◽  
...  
Keyword(s):  
Raw Materials ◽  
Chromatographic Determination ◽  
Raw Material ◽  
Liquid Chromatographic Method ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Amiodarone Hydrochloride ◽  
Related Compounds

Abstract A liquid chromatographic method for the determination of amiodarone hydrochloride and 10 related compounds in drug raw material and for assay of drug in tablets was developed. The method specifies a 3 jxm Hypersil nitrile column (150 × 4.6 mm), a mobile phase of 1 + 1 acetonitrile–ammonium acetate buffer (0.1 M adjusted to pH 6.0 with 0.1 M acetic acid), a flow rate of 1 mL/min, and detection at 240 nm. The lower limit of quantitation of the related compounds is 0.02% or less. Drug contents in 2 raw material samples were 100.1 and 99.9% and ranged from 98.2 to 99.4% in 3 tablet formulations. Impurity levels in 2 samples of raw material from different manufacturers were ca 0.4%. The presence of 3 of the known related compounds in these samples was confirmed by liquid chromatographymass spectrometry. The method applied to raw materials was evaluated by a second laboratory and found to be satisfactory.

Liquid Chromatographic Determination of Sulfentrazone in Soil

1999 ◽  
Vol 82 (5) ◽  
pp. 1214-1216 ◽  
Author(s):  
G Anthony Ohmes ◽  
Thomas C Mueller
Keyword(s):  
Chromatographic Determination ◽  
Soil Samples ◽  
Ultraviolet Detection ◽  
Liquid Chromatographic Separation ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Soluble Components

Abstract A rapid method for the determination of sulfentrazone in soils is described. The method consists of extraction of soil samples with methanol, filtration, liquid chromatographic separation of methanol-soluble components through a C18 column, and ultraviolet detection at 220 nm. Recoveries from fortified surface soils were >85% for sulfentrazone. Average relative standard deviations over the soils examined was 7.7%. A conservative lower limit of quantitation for sulfentrazone was 40 ng/g soil.

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 Benzoyl Peroxide in Acne Preparations

1984 ◽  
Vol 67 (5) ◽  
pp. 913-915
Author(s):  
Chih-Kuang Chou ◽  
David C Locke
Keyword(s):  
Benzoyl Peroxide ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Detector Response ◽  
Electrochemical Detector ◽  
Reverse Phase ◽  
Order Of Magnitude ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A rapid, precise, and accurate liquid chromatographic (LC) method is described for the determination of benzoyl peroxide (BP) in acne preparations. BP is extracted from a water dispersion of the preparation with dichloromethane (DCM), and an aliquot is eluted from a C-18 reverse phase LC column with acetonitrile-O.lOM aqueous NaCI04. Selective and sensitive quantitation is accomplished with a reductive mode electrochemical detector. This detector is an order of magnitude more sensitive than a 240 nm UV absorption detector; the lower limit of detection is 2 ng for a 4 μL injection. The recovery of BP is 99.4% and the detector response is linear to at least 2 μg per 4 μL injection.

scholarly journals Micellar Liquid Chromatographic Determination of Carbaryl and 1-Naphthol in Water, Soil, and Vegetables

2012 ◽  
Vol 2012 ◽  
pp. 1-7 ◽  
Author(s):  
Mei-Liang Chin-Chen ◽  
Maria Rambla-Alegre ◽  
Abhilasha Durgbanshi ◽  
Devasish Bose ◽  
Sandeep K. Mourya ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Cetylpyridinium Chloride ◽  
Sodium Dodecyl ◽  
Chromatographic Determination ◽  
Limit Of Quantification ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

A liquid chromatographic procedure has been developed for the determination of carbaryl, a phenyl-N-methylcarbamate, and its main metabolite 1-naphthol, using a C18 column (250’mm’ × ’4.6’mm) with a micellar mobile phase and fluorescence detection at maximum excitation/emission wavelengths of 225/333’nm, respectively. In the optimization step, surfactants sodium dodecyl sulphate (SDS), Brij-35 andN-cetylpyridinium chloride monohydrate, and organic solvents propanol, butanol, and pentanol were considered. The selected mobile phase was 0.15’M SDS-6% (v/v)-pentanol-0.01’M NaH2PO4buffered at pH 3. Validation studies, according to the ICH Tripartite Guideline, included linearity (r>0.999), limit of detection (5 and 18’ng mL-1, for carbaryl and 1-naphthol, resp.), and limit of quantification (15 and 50’ng mL-1, for carbaryl and 1-naphthol, resp.), with intra- and interday precisions below 1%, and robustness parameters below 3%. The results show that the procedure was adequate for the routine analysis of these two compounds in water, soil, and vegetables samples.

scholarly journals Liquid Chromatographic Determination of Fenbendazole Residues in Pig Tissues after Treatment with Medicated Feed

1999 ◽  
Vol 82 (5) ◽  
pp. 1007-1016 ◽  
Author(s):  
Bettencourt P S Capece ◽  
Belén Pérez ◽  
Eugeni Castells ◽  
Margarita Arboix ◽  
Carles Cristòfol
Keyword(s):  
High Performance ◽  
Chromatographic Determination ◽  
Farm Animals ◽  
Liquid Liquid Extraction ◽  
Limit Of Quantitation ◽  
Maximum Residue Limits ◽  
Cleanup Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Fenbendazole (FBZ) is an anthelmintic widely used in farm animals to treat parasitic infestations, in pigs, it is administered in the food. The aim of this study was to validate an analytical method for the determination of FBZ and its metabolites in pig tissues. This method is based on oxidation of FBZ and its sulfoxide metabolite to the sulfone metabolite (FBZSO2). The limit of quantitation for this method is 20 ng FBZSO2/g for all tissues. The maximum residue limits (MRLs) established for FBZ and its metabolites in pig tissues are 50 ng/g for muscle, fat, and kidney and 500 ng/g for liver. This method is based on a liquid-liquid extraction followed by an oxidation with peracetic acid and a cleanup procedure based on 2 liquid-liquid extractions. Determination is achieved by high- performance liquid chromatography with ultraviolet detection. The present method is adjusted to the MRL established for FBZ and its metabolite residues. The analysis of the residues shows that after 72 h posttreatment, no FBZSO2 was detected in muscle, fat, and kidney and that liver levels were below the MRL.

Gas-Liquid Chromatographic Determination of Azinphos Ethyl in Human Plasma and in Mouse Plasma, Tissue, and Fat

1976 ◽  
Vol 59 (5) ◽  
pp. 1094-1096
Author(s):  
Vincent B Stein ◽  
Kenneth A Pittman
Keyword(s):  
Human Plasma ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Tissue Samples ◽  
Mouse Plasma ◽  
Glass Column ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A new method for the determination of azinphos ethyl (O,O-diethyl-S-(4-oxo-1,2,3-benzotriazin-3(4H)-ylmethyl) phosphorodithioate) in human plasma and in mouse plasma, tissue, and fat has been developed. The method is based on extraction with benzene or hexane and cleanup of fat and tissue samples by a minicolumn containing Florisil and sodium sulfate. Azinphos ethyl is eluted from the column with 10% acetonitrile in benzene and is concentrated to an appropriate volume for gas-liquid chromatographic analysis, using a 63Ni electron capture detector and a glass column containing 3% OV-1 on Gas-Chrom Q. The method is sensitive to 0.005 ppm in human plasma, 0.01 ppm in mouse plasma, 0.08 ppm in mouse liver, 0.05 ppm in mouse brain, and 0.10 ppm in mouse fat. The limit of detection is 2 pg; mean recoveries ranged from 96 to 98%.

Matrix Solid-Phase Dispersion Extraction and Liquid Chromatographic Determination of Ivermectin in Bovine Liver Tissue

1992 ◽  
Vol 75 (4) ◽  
pp. 655-658 ◽  
Author(s):  
Frank J Schenck ◽  
Steven A Barker ◽  
Austin R Long
Keyword(s):  
Methylene Chloride ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Bovine Liver ◽  
Chromatographic Determination ◽  
Liver Sample ◽  
Antiparasitic Drug ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A method for the isolation and liquid chromatographic (LC) determination of the antiparasitic drug ivermectin in bovine liver is presented. Liver samples (0.5 g) are blended with 2 g C18 (octadecylsilylderivatized silica packing material). A column made from the C18liver matrix is washed with 3 mL hexane, then the ivermectin is eluted with methylene chloride-ethyl acetate (3 + 1). After purification by alumina solid-phase extraction, the ivermectin is derivatized and analyzed by LC with fluorescence detection. The overall recovery of ivermectin added to liver was 74.6%. The lowest level validated in tissue by the method was 10 ppb, and the limit of detection was 1 ppb. This method and a classical extraction method gave comparable results for a liver sample that contained incurred ivermectin residues. The method uses small volumes of solvents, has a limited number of sample manipulations, and does not require solvent partitioning or backwashing of extracts. These characteristics make this method attractive when compared to classical isolation procedures for ivermectin.

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