A high performance liquid chromatographic assay for the mycotoxin phomopsin A in lupin stubble

1987 ◽  
Vol 27 (1) ◽  
pp. 73 ◽  
Author(s):  
GR Hancock ◽  
P Vogel ◽  
DS Petterson

An assay using high performance liquid chromatography to measure phomopsin A, the principal mycotoxin responsible for lupinosis is described. Samples of lupin stubble are extracted with methanol: water and purified by partitioning between n-butanol and water, chromatography on Amberlite XAD-2 and by cation exchange chromatography. The analysis is performed on a reverse phase C18 column using a methanol:water gradient and UV detection. The limit of detection for this procedure is 0.5 mg phomopsin A per kg stubble. Improvements to the extraction and purification procedures were made and total analysis time was reduced to 2 days. The mean (� s.d.) recovery for the purification procedure was 64.3 � 4.5% over a wide range of concentrations.

2019 ◽  
Vol 11 (1) ◽  
pp. 216 ◽  
Author(s):  
Ramya Kuber B.

Objective: To develop a simple, sensitive, specific, accurate reverse phase high performance liquid chromatographic (RP-HPLC) method for the estimation of curcumin and piperine.Methods: The separation was done using a column Inertsil–ODS C18 (250 mm × 4.6 mm, 5µ particle size) and mobile phase composed of methanol: water (45:55 v/v), flow rate at 1 ml/min and detection was carried out at 282 nm with photodiode array (PDA) detector.Results: The separation of curcumin and piperine were found to be at the retention time of 2.433 min and 3.095 min, respectively. The method was found to be linear at a concentration range 20-80 µg/ml for curcumin and piperine. The limit of detection (LOD) and limit of quantification (LOQ) was found to be 0.05µg/ml and 0.17µg/ml for curcumin and 0.18µg/ml and 0.53µg/ml for piperine respectively. The average percentage recoveries of curcumin and piperine were in the range of 98-100.6%.Conclusion: A simple and sensitive reverse phase high performance liquid chromatographic method was developed for the estimation of curcumin and piperine.


1973 ◽  
Vol 1 (2) ◽  
pp. 387-390 ◽  
Author(s):  
R R Brodie ◽  
L F Chasseaud ◽  
E L Crampton ◽  
D R Hawkins ◽  
P C Risdall

A method has been developed for the separation and measurement of dothiepin and the N-desmethyl metabolite, northiaden, in human plasma or serum by high performance liquid chromatography. The method uses a structurally-related drug, amitriptyline, as an internal standard and provides a limit of detection of about 10 ng/ml for each component. At a concentration of 20 ng/ml, northiaden and dothiepin could be measured within ±11% and ± 6% of the mean respectively and at 200 ng/ml within ± 3% and ± 1% of the mean. The method has been applied to the analysis of serum from patients undergoing dothiepin therapy.


1983 ◽  
Vol 66 (3) ◽  
pp. 793-795
Author(s):  
Rodney J Bushway

Abstract This paper describes a reverse phase radial compression high performance liquid chromatographic (HPLC) method to determine rotenone in pesticide formulations. Formulations are extracted in dioxane by gentle swirling while sonicating for 5 min. A 10 μL aliquot is injected into the HPLC system equipped with a radial compression unit (Z module) containing a μBondapak C18 Radial-Pak column. The mobile phase is acetonitrile-methanol-tetrahydrofuranwater (34 + 30 + 1 + 35). Rotenone is monitored at 280 nm. Retention time for rotenone is approximately 7 min with total analysis time of 20 min. For 5 different products analyzed 11 times each, the percent coefficients of variation were all below 1.65. No interferences from 11 other rotenoids and 8 pesticides which are sometimes formulated with rotenone were observed.


1982 ◽  
Vol 39 (5) ◽  
pp. 778-782 ◽  
Author(s):  
V. K. Dawson

The high-performance liquid-chromatography (HPLC) procedure requires only minutes per sample, is specific, and is relatively sensitive (limit of detection < 0.005 mg/L for both chemicals). A combined buffer (pH 4) and internal standard (3-chlorodiphenylamine) reagent is added to the water sample, which is injected through a Sep Pak C18 disposable cartridge. The cartridge adsorbs and retains both the lampricides and the internal standard. The quantitative elution of the three chemicals from the cartridge with a small volume of methanol effectively concentrates the sample and provides sample cleanup. The methanol extract is then analyzed directly by HPLC on an MCH 10 reverse phase column by using a methanol:0.01 mol/L acetate buffer (87:13, v:v) as the mobile phase at 2 mL/min and detected by ultraviolet spectrophotometry at 330 (or 254) nm. A microprocessor data system further facilitates the procedure by quantifying off-scale peaks and yielding results directly in units of concentration (mg/L).Key words: sea lamprey, lampricides, methodology, chromatographic techniques, 3-trifluoromethyl-4-nitrophenol, 2′,5-dichloro-4′-nitrosalicylanilide, streams


INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (07) ◽  
pp. 32-37
Author(s):  
Vijaya Lakshmi Marella ◽  
Chaitanya S. N ◽  

A selective and sensitive reverse phase High Performance Liquid Chromatographic method has been developed and validated for the estimation of lornoxicam in bulk, pharmaceutical dosage forms and in dissolution samples. The analysis was performed isocratically on an Inertsil column (250* 4.6 mm, 5 µm) using a mass spectrometric compatible mobile phase of 10 mM ammonium acetate: acetonitrile (50:50 V/V) at a flow rate of 1 mL/min.The detection wavelength was 290 nm. The retention time was found to be 4.573 min for lornoxicam. The linearity of the method has been satisfied with Beer Lambert’s law in the concentration range of 5-25 µg/mL with a correlation coefficient of 0.9988. The mean recoveries assessed for lornoxicam were in the range of 100.39-101.86 %, indicating good accuracy of the method. The limit of detection and limit of quantification were found to be 0.03 and 0.11 µg/mL, respectively. The developed method has been statistically validated in accordance with ICH guidelines and found to be mass spectrometric compatible, simple, precise, and accurate with the prescribed values. Thus, the proposed method was successfully applied for the estimation of lornoxicam in routine quality control analysis of bulk, formulations and in dissolution samples.


Author(s):  
Bhupender Tomar ◽  
Ankita Sharma ◽  
Inder Kumar ◽  
Sandeep Jain ◽  
Pallavi Ahirrao

A simple, precise, and accurate reverse phase high performance liquid chromatographic method (RP-HPLC) was developed and validated for the estimation of the combination of 5- Fluorouracil (5-FU) and Imiquimod in active pharmaceutical ingredients (APIs). The method was carried out on Phenomenex C18 (250 × 4.6mm I.D., 5𝜇m) using isocratic elution mode. The mobile phase was used as Acetonitrile: 10mM potassium dihydrogen orthophosphate: triethylamine (40:59.9:0.1, v/v, pH 4.5 with orthophosphoric acid) and Water: ACN (50:50 v/v) was used as a diluent. The concentration of solvents was 1-20µg/ml and the volume of injection was 20µl with the flow rate of 1.2ml/min. The retention times for 5-FU and Imiquimod were found to be 1.9±0.5 and 6.6±0.5 min respectively. The absorption maxima of 5FU and Imiquimod were found 267nm and 227nm respectively. The method was validated as per ICH guidelines. All the data were found within the specified limits. The limit of detection (LOD) and limit of quantification (LOQ) of 5- Fluorouracil were found to be 0.015μg/mL and 0.048 μg/mL, respectively, and Imiquimod was found to be 0.078μg/mL and 0.237μg/mL, respectively. The method developed in the present study was found to be sensitive, specific, and precise and can be applied for the simultaneous estimation of 5-FU and Imiquimod.


INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (05) ◽  
pp. 48-52
Author(s):  
A Lodhi ◽  
◽  
A Jain ◽  
B. Biswal

A validated high performance liquid chromatographic method was developed for the determination of chromium picolinate in pharmaceutical dosage forms. The analysis was performed at room temperature using a reversed-phase ODS, 5µm (250×4.6) mm column. The mobile phase consisted of acetonitrile: buffer (60:40 V/V) at a flow rate of 0.5 mL/min. The PDA-detector was set at 264 nm. The developed method showed a good linear relationship in the concentration range from 1.5 – 12.5 µg/mL with a correlation coefficient from 0.999. The limit of detection and limit of quantification were 0.0540513 and 0.1637919 µg/mL respectively.


Sign in / Sign up

Export Citation Format

Share Document