Liquid Chromatographic Analysis System for Cyclopiazonic Acid in Peanuts

1984 ◽  
Vol 67 (4) ◽  
pp. 728-731 ◽  
Author(s):  
John A Lansden
Keyword(s):  
Limit Of Detection ◽  
Gaussian Model ◽  
Cyclopiazonic Acid ◽  
Detector Response ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Analysis ◽  
Modified Gaussian Model ◽  
Analysis System ◽  
Liquid Chromatographic ◽  
Exponentially Modified Gaussian

Abstract A liquid chromatographic procedure has been developed for analysis of cyclopiazonic acid in peanuts. The chromatographic system specifies a C18 or C8 column loaded with 4-dodecyldiethylenetriamine and an aqueous mobile phase containing 4-dodecyldiethylenetriamine, zinc acetate, ammonium acetate, 2-propanol, and acetonitrile. Cyclopiazonic acid was extracted from peanuts with methanol-chloroform (20 + 80), partitioned into aqueous sodium bicarbonate, acidified, and back-extracted into dichloromethane. The limit of detection (280 nm UV) was approximately 4 ng and detector response was linear to at least 1 μg pure cyclopiazonic acid. The recovery of cyclopiazonic acid from peanuts spiked at 68.9, 210, and 955 μ/kg was 85.9% (12.86% CV), 72.9% (6.43% CV), and 81.4% (0.40% CV), respectively. Calculation of the chromatographic peak parameters based on the exponentially modified Gaussian model indicated that the C18 column produced less peak skewing than did the C8 column.

scholarly journals Liquid Chromatographic Analysis of Vitamin K1 in Milk-Based Infant Formula with Matrix Solid-Phase Dispersion

1999 ◽  
Vol 82 (5) ◽  
pp. 1140-1145 ◽  
Author(s):  
G William Chase ◽  
Ronald R Eitenmiller ◽  
Austin R Long
Keyword(s):  
Infant Formula ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Reversed Phase ◽  
Vitamin K1 ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method for vitamin K1 in milk-based infant formula is described. The vitamins are extracted from infant formula by matrix solid-phase dispersion and quantitated by reversed-phase chromatography with fluorescence detection. Vitamin K1 is converted to the fluorescent hydroquinone with a postcolumn zinc reductive reactor. The limit of detection is 12 pg, and the limit of quantitation is 38 pg on-column. Linear responses were obtained in the range 0.55-22.1 ng/mL (r2 = 0.9998). Recoveries of vitamin K1 from an analyte-fortified blank material for milk-based infant formula averaged 91.7% (n = 25). The method provides a rapid, specific, and easily controlled assay for vitamin K1 in fortified infant formula.

scholarly journals Liquid Chromatographic Method for the Analysis of Brimonidine in Ophthalmic Formulations

2012 ◽  
Vol 9 (3) ◽  
pp. 1327-1331 ◽  
Author(s):  
A. Narendra ◽  
D. Deepika ◽  
M. Mathrusri Annapurna
Keyword(s):  
Limit Of Detection ◽  
Detector Response ◽  
Eye Drops ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Acid Sodium Salt ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

A reverse phase LC method was developed for the determination of Brimonidine in eye drops. Chromatography was carried on an Inertsil ODS 3V column (C18) using a mixture of Octane 1- sulfonic acid sodium salt (0.02M) (pH 3.5 ± 0.05) and acetonitrile (64:36 v/v) as mobile phase at a flow rate of 1 mL/min with UV detection at 254 nm. The drug was eluted at 4.636 min. The detector response was linear in the concentration range of 0.4–72 μg/mL. The limit of detection and limit of quantification were found to be 0.0561 and 0.1848 μg/mL respectively. The proposed method was validated as per the ICH guidelines and can be applied for the routine analysis of Brimonidine in eye drops.

scholarly journals Sensitive analysis of ethanolamine- and serine-containing phosphoglycerides by high-performance liquid chromatography

1975 ◽  
Vol 145 (3) ◽  
pp. 517-526 ◽  
Author(s):  
F B Jungalwala ◽  
R J Turel ◽  
J E Evans ◽  
R H McCluer
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Amino Groups ◽  
Tissue Samples ◽  
Primary Amino ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic

A highly sensitive method for the separation and quantitative measurement of phospholipids containing primary amino groups, such as phosphatidylethanolamine, phosphatidylserine and lysophosphatidylethanolamine, is described. The method involves a simple and quantitative derivative formation of the phospholipids containing amino groups to their u.v.-absorbing biphenylcarbonyl derivatives. These have molar extinction coefficients of about 23,000 at 268nm. The phospholipid derivatives are then separated and non-destructively determined by high-performance liquid chromatography. The amino phospholipids containing vinyl ether bonds (plasmalogens) can be determined separately from the diacyl- and alkylacyl-amino phospholipids. The lower limit of detection by high-performance liquid-chromatographic analysis of the phospholipid derivatives is about 10-13pmol or 0.3-0.4ng of phospholipid P. The quantitative range of derivative formation and analysis by high-performance liquid chromatography of the phospholipids containing amino groups was shown to be 10-500nmol. The method was shown to be applicable to the analysis of phospholipids containing amino groups in tissue samples.

Liquid-chromatographic analysis for serum theophylline in less than 70 seconds.

1982 ◽  
Vol 28 (4) ◽  
pp. 687-689 ◽  
Author(s):  
P M Kabra ◽  
L J Marton
Keyword(s):  
Chromatographic Analysis ◽  
High Speed ◽  
Limit Of Detection ◽  
Flow Cell ◽  
Reversed Phase ◽  
Serum Theophylline ◽  
Analytical Recovery ◽  
Micro Flow ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic

Abstract We describe a sensitive, specific, and very fast liquid-chromatographic assay for serum theophylline, involving a commercially available high-speed reversed-phase column and a micro-flow-cell-equipped detector. Each analysis requires only 100 microL of serum (as little as 25 microL may be used when necessary), and chromatography is complete in less than 70 s. Analytical recovery of theophylline added to serum ranged from 97 to 102%. Between-run precision (CV) ranged from 2.1 to 3.5%. The lower limit of detection for theophylline is 0.5 mg/L, and linearity extends to 50 mg/L. Numerous drugs and xanthine metabolites tested do not interfere.

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.

Fluorometric determination of indocyanine green in plasma.

1987 ◽  
Vol 33 (6) ◽  
pp. 765-768 ◽  
Author(s):  
B Hollins ◽  
B Noe ◽  
J M Henderson
Keyword(s):  
Indocyanine Green ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Biological Fluids ◽  
Complete Analysis ◽  
Spectrophotometric Methods ◽  
Specificity And Sensitivity ◽  
Order Of Magnitude ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic

Abstract With this fluorometric method for measuring indocyanine green (ICG) in biological fluids, the limit of detection is an order of magnitude lower than for the traditional spectrophotometric procedure. The excitation and emission maxima are 780 and 810 nm, respectively. Agreement was excellent (r = 0.998) between direct results by this method and those by a liquid-chromatographic procedure with spectrophotometric detection. ICG breaks down in aqueous solution; the degradation products can be detected with liquid-chromatographic/spectrophotometric methods, but because the metabolites are not fluorescent, they do not interfere in the method present here. The increased specificity and sensitivity of this method should permit much more complete analysis of the kinetics of ICG disposition.

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%.

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